Day: December 2, 2020

144690-92-6, A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.144690-92-6. An updated downstream synthesis route of 144690-92-6 as follows.

Example 2 Olmesartan medoxomil of formula I20 g of the starting compound of formula III were stirred up in 75 ml of acetic acid and after stirring for 10 minutes 30 ml of water were added dropwise during 5 minutes. Then, the suspension was put in a 50C bath and stirred for 4 hours. Then 16 ml of water were added dropwise in 5 minutes, the mixture was taken out of the bath and after 5 minutes it was put in a cooling bath with the temperature of 10C. After 20 minutes the separated insoluble fraction, containing the side product trityl alcohol, was aspirated and washed with a mixture of 4 ml of AcOH + 2 ml of water. 40 ml of acetone and then 70 ml of water were added to the filtrate at 30C, the separated product was aspirated and 1 1.5 g (82 %) of the product were obtained., 144690-92-6

Elementary reactions that involve the simultaneous collision of more than three molecules are highly improbable and have never been observed experimentally.

Reference£º
Patent; ZENTIVA, K. S.; STACH, Jan; JARRAH, Kamal; KRULIS, Radim; RADL, Stanislav; CERNY, Josef; WO2012/55380; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.144690-92-6. A new synthetic method of this compound is introduced below.

Example 2 Olmesartan medoxomil of formula I20 g of the starting compound of formula III were stirred up in 75 ml of acetic acid and after stirring for 10 minutes 30 ml of water were added dropwise during 5 minutes. Then, the suspension was put in a 50C bath and stirred for 4 hours. Then 16 ml of water were added dropwise in 5 minutes, the mixture was taken out of the bath and after 5 minutes it was put in a cooling bath with the temperature of 10C. After 20 minutes the separated insoluble fraction, containing the side product trityl alcohol, was aspirated and washed with a mixture of 4 ml of AcOH + 2 ml of water. 40 ml of acetone and then 70 ml of water were added to the filtrate at 30C, the separated product was aspirated and 1 1.5 g (82 %) of the product were obtained., 144690-92-6

There are, however, a few established termolecular elementary reactions. The reaction of nitric oxide with oxygen appears to involve termolecular steps.

Reference£º
Patent; ZENTIVA, K. S.; STACH, Jan; JARRAH, Kamal; KRULIS, Radim; RADL, Stanislav; CERNY, Josef; WO2012/55380; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.Triphenyl methyl olmesartan, cas is 144690-92-6. Here is a downstream synthesis route of the compound 144690-92-6, 144690-92-6

To the three-necked flask were added with 38 ml of ethyl acetate, 45 g of 6.4% dilute hydrochloric acid, 25 g of trityl olmesartan medoxomil was added with stirring. Stir in water bath, control the temperature 15 to 20 C, stirring about 4 hours, TLC plate detection point of raw material disappeared,That is, it is judged that the deprotection reaction is completed.Cooled to room temperature, 115 ml * 5 toluene was added to wash, the aqueous layer was added with 135 ml of acetone, potassium bicarbonate aqueous solution adjusted P=4.0, control temperature 15 ¡À 5 C Stir for 2 hours, Filtered and dried to give 16.0 g of olmesartan medoxomil in a yield of 90.2%. HPLC analysis: purity 98.75%, impurity a (olmesartan acid) 0.71%, individual impurities less than 0.10%

144690-92-6 is used more and more widely, we look forward to future research findings about Triphenyl methyl olmesartan

Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd,; Huang, Xiangliang; Zhang, LI; Hua, yuanyuan; Wu, Yong De; (7 pag.)CN102584804; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.144690-92-6. A new synthetic method of this compound is introduced below.

To the three-necked flask were added with 38 ml of ethyl acetate, 45 g of 6.4% dilute hydrochloric acid, 25 g of trityl olmesartan medoxomil was added with stirring. Stir in water bath, control the temperature 15 to 20 C, stirring about 4 hours, TLC plate detection point of raw material disappeared,That is, it is judged that the deprotection reaction is completed.Cooled to room temperature, 115 ml * 5 toluene was added to wash, the aqueous layer was added with 135 ml of acetone, potassium bicarbonate aqueous solution adjusted P=4.0, control temperature 15 ¡À 5 C Stir for 2 hours, Filtered and dried to give 16.0 g of olmesartan medoxomil in a yield of 90.2%. HPLC analysis: purity 98.75%, impurity a (olmesartan acid) 0.71%, individual impurities less than 0.10%

There are, however, a few established termolecular elementary reactions. The reaction of nitric oxide with oxygen appears to involve termolecular steps.

Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd,; Huang, Xiangliang; Zhang, LI; Hua, yuanyuan; Wu, Yong De; (7 pag.)CN102584804; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

37830-90-3, A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.37830-90-3. An updated downstream synthesis route of 37830-90-3 as follows.

Add 50.0 g of 4,5-dimethyl-1,3-dioxol-2-one to a 1 L four-necked flask.530 g of dichloromethane, stirred and dissolved, and heated to reflux, when the internal temperature is not lower than 40 ¡ã C,A mixture of 65 g (1.1 equivalents) of sulfonyl chloride and 132 g of dichloromethane was added dropwise.The internal temperature of the control is not lower than 40 ¡ãC, and the mixture is kept warm for 2 hours after the dropwise addition.The temperature was then raised to 85 ¡ã C while distilling off the dichloromethane. When it reaches 85 ¡ã C, it is rearranged for 2 to 3 hours.At room temperature, crude DMDO-Cl was obtained with a GC purity of 85percent to 90percent.Add 30 ml of isopropanol to the above crude product, stir and cool to -10 ¡ã C ~ -5 ¡ã C,Crystallization 0 ~ 1h, suction filtration, rinse with isopropanol down to -5 ¡ã C,Obtained white crystals 53.3g (yield 81.9percent, GC purity 99.3percent)

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; Zhejiang Huahai Pharmaceutical Co., Ltd.; Wang Jiquan; Li Guoxiang; Xiong Xueqiang; (6 pag.)CN103864748; (2019); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.4,5-Dimethyl-1,3-dioxol-2-one, cas is 37830-90-3. Here is a downstream synthesis route of the compound 37830-90-3, 37830-90-3

Add 50.0 g of 4,5-dimethyl-1,3-dioxol-2-one to a 1 L four-necked flask.530 g of dichloromethane, stirred and dissolved, and heated to reflux, when the internal temperature is not lower than 40 ¡ã C,A mixture of 65 g (1.1 equivalents) of sulfonyl chloride and 132 g of dichloromethane was added dropwise.The internal temperature of the control is not lower than 40 ¡ãC, and the mixture is kept warm for 2 hours after the dropwise addition.The temperature was then raised to 85 ¡ã C while distilling off the dichloromethane. When it reaches 85 ¡ã C, it is rearranged for 2 to 3 hours.At room temperature, crude DMDO-Cl was obtained with a GC purity of 85percent to 90percent.Add 30 ml of isopropanol to the above crude product, stir and cool to -10 ¡ã C ~ -5 ¡ã C,Crystallization 0 ~ 1h, suction filtration, rinse with isopropanol down to -5 ¡ã C,Obtained white crystals 53.3g (yield 81.9percent, GC purity 99.3percent)

A chemical reaction often occurs in steps, although it may not always be obvious to an observer.

Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd.; Wang Jiquan; Li Guoxiang; Xiong Xueqiang; (6 pag.)CN103864748; (2019); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

One of the major reasons is to use measurements of the macroscopic properties of a system, the rate of change in the concentration of reactants or products with time, to discover the sequence of events that occur at the molecular level. 80841-78-7, introduce a new downstream synthesis route. 80841-78-7

123.2g of compound and 2.5g of potassium hydroxide solid were added to a 500ml four-necked flask.DMAC76g, heated to 50 C, stirred for about 6h,The TLC dot plate showed that the compound 1 point disappeared, that is, the end of the hydrolysis reaction was judged.Cool to 15 ¡À 5 C, add KBr 0.64g, add DMDO-C16.5g, DMAC 10g,After about 40 minutes, the temperature was raised to 25¡À5C for 2h, then the temperature was raised to 50C, the reaction was about 6h, and the temperature was lowered again to 20¡À5C for 5h. The reaction solution was added with 324g water and 208g of dichloromethane.Shake well and let the layers separate. The aqueous layer was extracted with 70 g of dichloromethane and combined with several layers.It was washed twice with 206 g of water, and the last aqueous layer was extracted with 100 g of dichloromethane.The organic layers were combined and dried under reduced pressure at 45 C.After adding 100g of the upper batch of crystallization, the mother liquid is heated and refluxed for 25¡À5 minutes, and then naturally cooled.Then crystallization at 0 C for 6 h,Drying by suction filtration to obtain 23.2 g of trityl olmesartan medoxomil white solid powder.The yield was 93.4%. HPLC analysis, purity 99.7%, acid miscellaneous <0.05%,The olefinic impurity is <0.1%, and the other unknown single impurities are <0.1%. There are, however, a few established termolecular elementary reactions. The reaction of nitric oxide with oxygen appears to involve termolecular steps. Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd.; Xiong Xueqiang; Li Guoxiang; Wang Jiquan; (6 pag.)CN103880825; (2019); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.80841-78-7, molecula formula is 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, below Introduce a new synthetic route., 80841-78-7

123.2g of compound and 2.5g of potassium hydroxide solid were added to a 500ml four-necked flask.DMAC76g, heated to 50 C, stirred for about 6h,The TLC dot plate showed that the compound 1 point disappeared, that is, the end of the hydrolysis reaction was judged.Cool to 15 ¡À 5 C, add KBr 0.64g, add DMDO-C16.5g, DMAC 10g,After about 40 minutes, the temperature was raised to 25¡À5C for 2h, then the temperature was raised to 50C, the reaction was about 6h, and the temperature was lowered again to 20¡À5C for 5h. The reaction solution was added with 324g water and 208g of dichloromethane.Shake well and let the layers separate. The aqueous layer was extracted with 70 g of dichloromethane and combined with several layers.It was washed twice with 206 g of water, and the last aqueous layer was extracted with 100 g of dichloromethane.The organic layers were combined and dried under reduced pressure at 45 C.After adding 100g of the upper batch of crystallization, the mother liquid is heated and refluxed for 25¡À5 minutes, and then naturally cooled.Then crystallization at 0 C for 6 h,Drying by suction filtration to obtain 23.2 g of trityl olmesartan medoxomil white solid powder.The yield was 93.4%. HPLC analysis, purity 99.7%, acid miscellaneous <0.05%,The olefinic impurity is <0.1%, and the other unknown single impurities are <0.1%. There are, however, a few established termolecular elementary reactions. The reaction of nitric oxide with oxygen appears to involve termolecular steps. Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd.; Xiong Xueqiang; Li Guoxiang; Wang Jiquan; (6 pag.)CN103880825; (2019); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.80841-78-7. An updated downstream synthesis route of 80841-78-7 as follows.

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

80841-78-7, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.80841-78-7. A new synthetic method of this compound is introduced below.

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.

There are, however, a few established termolecular elementary reactions. The reaction of nitric oxide with oxygen appears to involve termolecular steps.

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