Tag: M.W:800-900

In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 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%

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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

In heterogeneous catalysis, the catalyst is in a different phase from the reactants. 144690-92-6, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 144690-92-6, name is C48H44N6O6. In an article£¬Which mentioned a new discovery about 144690-92-6

To 12.0g (15 mmol) of tritylolmesartan medoxomil prepared according to examples 1 or 2 69 ml of ethyl acetate was added and after that 12 ml of methanol and 2.67 ml (32 mmol) of conc. HCl were added. The mixture was stirred at room temperature for 2h and then the mixture was cooled to below 2C. To the cooled mixture 71 ml of 1% NH3 was slowly added to adjust pH to 4.93. The phases were separated and water phase was reextracted with 20 ml of ethyl acetate. Collected organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure to approximately 15g of oily residue. To this residue 15 ml of ethyl acetate were added and the mixture was cooled to 20 C and stirred at this temperature for 2h, and then cooled under 0C and stirred at this temperature for 1hour. The product was filtered off and washed with 5 ml of fresh ethyl acetate and dried. Yield: 7.55 g (90%). HPLC: 99.81 % of the product, all individual impurities under 0.10%.

The catalyzed pathway has a lower Ea, but the net change in energy that results from the reaction is not affected by the presence of a catalyst. In my other articles, you can also check out more blogs about Triphenyl methyl olmesartan.C48H44N6O6

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Patent; Krka Tovarna Zdravil, D.D., Novo Mesto; EP2334668; (2011); A1;,
1,3-Benzodioxole – Wikipedia
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In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 144690-92-6

A solution of MTT in 10 volumes of acetic acid (75%) was heated for 1.5 hrs at 60 C. until a pH of 2.21-2.23 was achieved, 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.)., 144690-92-6

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

In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 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

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

In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 144690-92-6

Into a 1000 mL four-necked flask equipped with a two-piece stirring blade having a diameter of 10 cm,50 g of trityl olmesartan medoxomil, 225 ml of acetic acid and 75 ml of water were added and stirred at 40 C. for 2 hours to carry out deprotection reaction.Subsequently, the reaction solution was cooled to 20 C. and stirred at 20 C. for 1 hour, and the precipitated triphenylmethanol was removed by vacuum filtration,To the obtained filtrate were added 250 ml of 10% sodium hydrogen carbonate and 500 ml of ethyl acetate, followed by vigorous stirring, and the aqueous layer was separated to obtain an organic layer containing olmesartan medoxomil.200 ml of ethyl acetate was distilled off from the organic layer, and the mixture was stirred at 20 to 30 C. for 1 hour. The precipitated solid was collected by filtration under reduced pressure as a wet body.The obtained wet body was dried at 40 C. for 14 hours to obtain 30 g of crystals of olmesartan medexomil (purity: 99.54%)., 144690-92-6

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Reference£º
Patent; TOKUYAMA CORPORATION; MORI, HIROYUKI; TANAKA, KENJI; (11 pag.)JP2015/74608; (2015); A;,
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144690-92-6,Chemistry, like all the natural sciences, begins with the direct observation of nature¡ª in this case, of matter. Which mentioned a new discovery about 144690-92-6.

Example 7:Preparation of olmesartan medoxomil Trityl olmesartan medoxomil (260 gm) as obtained in example 1 was dissolved in toluene (2600 ml) and then added concentrated hydrochloric acid (156 ml) for 1 hour 30 minutes at room temperature. The reaction mass was maintained for 1 hour 30 minutes at room temperature and then added water (1000 ml). The reaction mass was stirred for 45 minutes at room temperature and the layers were separated. To the aqueous layer was added ethyl acetate (5000 ml) at room temperature. The reaction mass was cooled to 15 to 20C and pH of the reaction mass was adjusted to 4.5 to 5.5 with sodium carbonate (20%, 560 ml). The reaction mass was stirred for 20 minutes at 20C and the layers were separated. The organic layer was dried over sodium sulfate and ethyl acetate was distilled off completely under vacuum at below 45C to obtain a residual mass. To the residual mass was added ethyl acetate (400 ml) at 40C and then heated to 75 to 80C. The contents were maintained for 30 minutes at 75 to 80C. The reaction mass was cooled to room temperature and stirred for 1 hour. The reaction mass was further cooled to 10 to 15C and stirred for 1 hour 30 minutes, filtered. The solid obtained was dried at 40 to 45C for 4 hours to obtain 150 gm of olmesartan medoxomil.Olmesartan medoxomil: 98.6%;Olmesartan acid impurity: 0.32%;Trityl olmesartan medoxomil impurity: 0.35%Methyl olmesartan medoxomil impurity: 0.35%.

Note that a catalyst decreases the activation energy for both the forward and the reverse reactions and hence accelerates both the forward and the reverse reactions.144690-92-6, you can also check out more blogs about144690-92-6

Reference£º
Patent; HETERO RESEARCH FOUNDATION; PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; MURALIDHARA REDDY, Dasari; RAJI REDDY, Rapolu; RAMAKRISHNA REDDY, Matta; VAMSI KRISHNA, Bandi; WO2012/1694; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6,Chemistry, like all the natural sciences, begins with the direct observation of nature¡ª in this case, of matter. Which mentioned a new discovery about 144690-92-6.

A 250 round bottom flask was loaded with MTT (10 g), acetone/water (2/2 vol.), and 3 eq of H2SO4. The mixture was stirred at 40 C., and after 2-4 hrs, triphenyl carbinol (TPC) was precipitated by the addition of water and filtrated out. NaHCO3 was added to the filtrate and the mixture was cooled to room temperature and stirred for 1 hr. Crude olmesartan medoxomil was obtained as white crystals (90% yield).

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Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; US2006/149078; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In heterogeneous catalysis, the catalyst is in a different phase from the reactants. 144690-92-6, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 144690-92-6, name is C48H44N6O6. In an article£¬Which mentioned a new discovery about 144690-92-6

Example 4; Olmesartan medoxomil (V); The starting substance (III; 10 g) was dissolved in acetone (50 ml), and, after adding water (25 g), the mixture was heated to a mild boil for 14 h. After evaporating acetone and adding ethyl acetate (50 ml), water was separated, and the organic layer was again washed with water (10 ml). The extract was concentrated and evaporated with toluene (50 ml) once more, the residue was dissolved in ethyl acetate (20 ml) and toluene (20 ml). The mixture was concentrated to 25 ml and allowed to crystallize under stirring for 30 min; after cooling to 15 C, the insoluble portion was sucked off and washed with ethyl acetate. 6.5 g of the product was obtained, which, after recrystallization from ethanol, gave 6 g (86 %) of the product with an HPLC purity of 98.7 %.By further recrystallization from ethyl acetate and cyclohexane, 5.1 g of a sample with an HPLC purity of 99.6 % was obtained. 1H NMR (250 MHz, CDCl3) delta: 0.82 (3H, t, J = 7.5 Hz); 1.50 (6H, s); 1.54-1.63 (2H, m); 2.07 (3H, s); 2.48 (2H, t, J = 7.5 Hz); 4.86 (2H, s); 5.32 (2H, s); 6.70 (2H, d, J = 8 Hz); 6.99 (2H, d, J = 8 Hz); 7.3-7.5 (3H, m); 7.72 (IH, dd, J = 1.7 Hz).

The catalyzed pathway has a lower Ea, but the net change in energy that results from the reaction is not affected by the presence of a catalyst. In my other articles, you can also check out more blogs about Triphenyl methyl olmesartan.C48H44N6O6

Reference£º
Patent; ZENTIVA, A.S.; WO2007/48361; (2007); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In heterogeneous catalysis, the catalyst is in a different phase from the reactants. 144690-92-6, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 144690-92-6, name is C48H44N6O6. In an article£¬Which mentioned a new discovery about 144690-92-6

10L reaction flask was charged 500.0g (0.62mol) compound 6,3L water, 1L of acetone, was added dropwise a solution of 645.0g of 22.5% sulfuric acid at 20 . Dropping was completed, the reaction at room temperature after 4.5h TLC or HPLC in control, raw reaction was complete. Body cooling system to 0-5 , when the temperature stabilized filtrate back into the reaction vessel was charged with acetone 1L and 2L water. The system was maintained at 15 solution of 210g of potassium carbonate and 400g water to form a solution, drops of completion, stirring after 1-2h incubation filtration. The filter cake was dried to obtain olmesartan medoxomil pure 328.9g. HPLC: 99.96%, yield: 94.3%, 144690-92-6

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Reference£º
Patent; Jiangsu Bang Pharmaceutical Co., Ltd.; Zhao, Guangrong; Huan, Shuang; Zhao, Huayang; Liu, Liping; Chen, Guoping; Tang, Jingyu; (19 pag.)CN105481842; (2016); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In heterogeneous catalysis, the catalyst is in a different phase from the reactants. 144690-92-6, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 144690-92-6, name is C48H44N6O6. In an article£¬Which mentioned a new discovery about 144690-92-6

The reaction flask was charged with 400 g of compound VII (0.50 mol) and 70% aqueous acetic acid solution of 3200 ml, Reaction was carried out at 50 C for 2 hours. After the completion of the reaction, the solvent was concentrated and concentrated, and ammonia was added to the residue.PH = 7, extracted with 1400 ml of ethyl acetate, the ethyl acetate layer was washed with water, and finally with anhydrous sodium sulfateDried; filtered, the filtrate was concentrated to dryness and the residue was recrystallized from ethanol to give the compound I pure product 256.1G, yield: 91.79%.

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Reference£º
Patent; Hunan Ouya biological Co. Ltd.; Lin, kaizhao; (19 pag.)CN103304550; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem