Dioxole related

144690-92-6, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”144690-92-6

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5, 144690-92-6

As the rapid development of chemical substances, we look forward to future research findings about 144690-92-6

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”144690-92-6

To TOLM (75 g) were successively added acetic acid_water=1:1 (330 mL, 4.4 vol) and concentrated sulfuric acid (5.4 mL, 1.08 eq). The obtained mixture was stirred at 25C – 30C for 1 hr. Using TLC (thin layer chromatography) (TLC eluent: 10% methanol/methylene chloride, detection method: UV), complete disappearance of TOLM was confirmed. [0309] The reaction mixture was filtered and insoluble trityl alcohol was removed. The aqueous layer was adjusted to pH 2 – 3 by adding 25% aqueous sodium carbonate solution (initial pH of the reaction mixture was 4 – 4.5). The reaction mixture was stirred for 5 min, methylene chloride (225 mL, 3 vol) was added thereto, and the mixture was stirred for 5 min. Stirring was stopped, and the mixture was stood and partitioned. The aqueous layer was extracted with methylene chloride (2×225 mL, 2×3 vol), the extracts were combined with the organic layer, deionized water (375 mL, 5vol) was added, and the mixture was stirred for 5 min. Stirring was stopped, and the mixture was stood for 5 min and partitioned. To the organic layer was added saturated brine (375 mL, 5 vol), and the mixture was stirred for 5 min, left standing and partitioned. The organic layer was concentrated under reduced pressure at 40C – 45C to give crude OLM MDX (49 g, 93%) as a pale-yellow solid.To the crude OLM MDX (49 g, 1 eq) obtained in the above-mentioned (7) was added acetone (735 mL, 15 vol), and the mixture was stirred at 55C – 60C for 10 min. Furthermore, the reaction mixture was stirred at the same temperature for 15 min, and acetone was evaporated under normal pressure. Heating was stopped when a solid was precipitated, and the mixture was cooled to 25C – 30C. The precipitated solid was collected by filtration and dried with suction for 30 min to give OLM MDX (41 g, 83%). [0311] To the OLM MDX obtained above was added isopropyl alcohol (164 mL, 4 vol), and the mixture was heated to 55C – 60C, and stirred at 55C – 60C for 1 hr. Heating was stopped and the mixture was gradually cooled to 25C – 30C, and stirred at 25C – 30C for 30 min. The precipitated solid was filtered and dried with suction to give OLM MDX (41 g, 100%). [0312] The OLM MDX (41 g) obtained above and acetone (about 1 L) were heated to 55C – 60C, and stirred at 55C – 60C for 25 min. Acetone was evaporated under normal pressure until the mixture became cloudy, and the mixture was gradually cooled to 25C – 30C. The precipitated solid was collected by filtration and dried with suction for 30 min to give OLM MDX (34 g, 83%). The HPLC purity of the obtained OLM MDX was 99.66%. [0313] The OLM MDX (44 g) obtained above was dissolved in acetone (about 1.2 L), and the mixture was stirred at 55C-60C for 10 min. Acetone was evaporated under normal pressure until the solution became cloudy, and the solution was gradually cooled to 25C – 30C. The precipitated solid was collected by filtration, dried with suction for 30 min, blast dried for 1 hr, and further blast dried at 40C – 45C for 5 hr to give OLM MDX (36 g) as a white solid. The HPLC purity of the obtained OLM MDX was 99.8%.

The chemical industry reduces the impact on the environment during synthesis, Triphenyl methyl olmesartan, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; API Corporation; SEKI, Masahiko; EP2891650; (2015); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

EXAMPLE 1 Preparation of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) To a solution of 50 g of 4,5-dimethyl-1,3-dioxolene-2-one (IV)(Synthesised by the method described in Tetrahedron Letters, 1701-1704 (1972)) in 350 ml of methylene chloride was added 65 g of sulfuryl chloride dropwise over 1 hour at 40¡ã-42¡ã C. The mixture was stirred for one hour at the same temperature and then evaporated in vacuo to remove the solvent. The resulting residue was distilled in vacuo to obtain 42.1 g (65percent of theory) of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) as a colorless oil. B.p. 45¡ã-48¡ã C./2 mmHg. IR(CHCl3)nu(cm-1): 1820, near 1695 etc. NMR(CDCl3, delta(ppm)): 2.19(3H, s, CH3), STR5

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; Kanebo, Ltd.; US4554358; (1985); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

To a solution of the compound of Formula IV (5.0 g) in toluene (40 mL), dimethylacetamide (10 mL) is added, followed by addition of sodium hydroxide (1.2 g) and N,N-diisopropylamine (3.7 g) at 25-35C. The mixture is stirred at 40- 45C for 4 hours. 5-Methyl-2-oxo-(1 ,3-dioxolene-4-yl)methyl chloride (1.5 g) and tetrabutylammonium bromide (0.5 g) are added at 40-450C. The mixture is stirred at 60-70C for 8 hours. The mass is cooled to 25-35C, water (50 mL) is added, and the pH is adjusted to about 6-7 by adding 10% aqueous HCI. The layers are separated. The aqueous layer is extracted with toluene (25 mL). The organic layers are combined and washed with water (25 mL). The solvent is distilled under reduced pressure. Methanol (25 mL) is added to the residue. The mixture is cooled to 0-50C and stirred at that temperature for 45 minutes. The formed solid is filtered, washed with methanol (10 mL) and dried for 45 minutes under vacuum (yield 3.0 g).

The chemical industry reduces the impact on the environment during synthesis, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; KOLLA, Naveen Kumar; MANNE, Nagaraju; NAREDLA, Anitha; SHINDE, Sachin Gulabrao; WO2011/14611; (2011); A2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”144690-92-6

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5

The chemical industry reduces the impact on the environment during synthesis, Triphenyl methyl olmesartan, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.144690-92-6, Triphenyl methyl olmesartan it is a common compound, a new synthetic route is introduced below.144690-92-6

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Triphenyl methyl olmesartan reaction routes.

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

To the flask was added 2000 g of acetone, 160 g of ethyl 4- (1-hydroxy-1-methylethyl) -2-propylimidazole-5-carboxylate (II), 150 g of K2CO3, 460 g of 4- [2- (Trityltetrazol-5-yl) phenyl] benzyl bromide (III), 20g KI, the temperature was raised to reflux, the reaction was incubated for 34-38 hours under stirring.Then add 102g KOH, reflux reaction 6 ~ 8h. Cool to 10 ~ 20 , add 170g DMDO-Cl, incubated for 30 ~ 60min.Heating to reflux, the reaction 22 to 26 hours.After the reaction was added 40g of diatomaceous earth, stirring for 30 to 60 minutes, suction filtration, 200g acetone rinse cake. To the filtrate was added 800g of drinking water and 200g of refined hydrochloric acid, the reaction at room temperature for 2 to 4 hours, filtered to remove by-product triphenylcarbinol. Dropping 10% K2CO3 aqueous solution, adjusting feedstock pH to 4, cooling to 10 ~ 20 , stirring crystallization 2h, filtration, the filter cake with a mixture of pre-cooled 45g acetone and 230g of drinking water washing and drying, to obtain Olmesartan Medoxomil 309 g, total yield 83.1% (relative to ethyl-4- (1-hydroxy-1-methylethyl) -2-propylimidazole-5- carboxylate (II)), purity: 99.27% of the main peak, 0.08% of the olmesartan acid, 0.14% of the triphenylmethanol, and 0.13% of the largest unidentified one.

The chemical industry reduces the impact on the environment during synthesis, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Zhejiang Huahai Zhicheng Pharmaceutical Co., Ltd.; Zhejiang Huahai Pharmaceutical Co., Ltd.; Jin Congyang; Wang Jiquan; Zhang Wenling; Wang Peng; (10 pag.)CN107311990; (2017); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”144690-92-6

Example 1323.88 g of (V) were suspended in 92 ml of acetonitrile. The mixture was cooled to 5C in order to add 24.6 ml of 6N HCI. The mixture was stirred for 2 hours at 5C. 150 ml of toluene were added. The pH was adjusted to 5.7 with potassium bicarbonate. The mixture was filtered in order to eliminate part of the salts generated. The solid was washed with 30 ml of acetonitrile. The phases were separated. The acetonitrile present in the organic phase was distilled. The mixture was cooled and filtered. The solid was washed with toluene and water. (VI) was dried in a heat cabinet. 16.66 g of (VI) were obtained (85% yield).

The chemical industry reduces the impact on the environment during synthesis, Triphenyl methyl olmesartan, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; INTERQUIM, S.A.; JOVE MARTI, Iban; MARQUILLAS OLONDRIZ, Francisco; WO2012/55994; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

To a stirred solution of 4, 5-dimethyl-l, 3-dioxol-2-one (4.5 g, 39.4 mmol) in benzene (150 mL), were added NBS (15.44 g, 87 mmol) and AIBN (0.648 g, 3.94 mmol). The reaction mixture was stirred at 1 10 C for 2 h under nitrogen atmosphere and subsequently concentrated in vacuo. The residue was dissolved in ethyl acetate (200 mL). The solution was washed with water (2* 150 mL) and brine (100 mL), dried over anhydrous sodium sulphate and concentrated in vacuo to get the crude product as a light brownish oil, which was purified by CombiFlash chromatography (60-120 silica gel; 5- 55% ethyl acetate in pet. ether as eluent) to afford 4,5 -bis (bromomethyl)-l,3-dioxol-2- one (7 g, 66%) as a light yellowish oil. NMR (400 MHz, Chloroform-7) d ppm 4.22 (s, 4H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; BRISTOL-MYERS SQUIBB COMPANY; BALOG, James Aaron; SEITZ, Steven P.; WILLIAMS, David K.; ANDAPPAN MURUGAIAH SUBBAIAH, Murugaiah; (191 pag.)WO2019/136112; (2019); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”144690-92-6

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5, 144690-92-6

As the rapid development of chemical substances, we look forward to future research findings about 144690-92-6

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem