Category: 144690-92-6

144690-92-6,In homogeneous catalysis, the catalyst is in the same phase as the reactant. The number of collisions between reactants and catalyst is at a maximum.In a article,Triphenyl methyl olmesartan,introducing its new discovery.

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
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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

Take 40g of compound 5, Add 80mL of methanol, 330 mL of ethyl acetate, Warmed to 45 , After 8 hours of reaction, Add 860mL water, Insoluble matter was removed by filtration, The filtrate was concentrated, In oily liquid, Acetonitrile, Stirred under a solid precipitation, filter, Washed with ethanol, 23.2 g of white solid was obtained, The yield was 83.1% The HPLC purity was 99.2%.

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Patent; Disha Pharmaceutical Group Co., Ltd.; Zhang Zhaoxing; Zhang Hongqiang; Qin Litai; Li Wei; Li Zongwen; Xia Haijian; (6 pag.)CN103012382; (2016); B;,
1,3-Benzodioxole – Wikipedia
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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 1-6 (0333) (0334) A mixture of TOLM (0.6 g, 0.75 mmol), sulfuric acid (0.08 g, 0.82 mmol) and 1:1 water-containing acetic acid (2.6 mL, 4.3 vol) was stirred at 25 C. for 1 hr. The reaction mixture was filtered, and the obtained solid was washed with 1:1 water-containing acetic acid (6.0 mL, 10 vol). The filtrates were combined and adjusted to pH 4-5 by adding 25% aqueous sodium carbonate solution. The mixture was partitioned by adding methylene chloride (6.0 mL, 10 vol). The aqueous layer was extracted with methylene chloride (3¡Á5 mL). The organic layer was washed with water (2¡Á5 mL) and saturated brine (5 mL), and concentrated under reduced pressure. The concentrated residue was purified by silica gel column chromatography (5-6% methanol/methylene chloride) and recrystallized from acetonitrile to give OLM (0.45 g, yield 100%). (0335) melting point: 174.5 C.-175.2 C.; (0336) IR (KBr): numax=2969, 1831, 1706, 1475, 1226, 1134, 760 cm-1; (0337) 1H NMR (DMSO-d6): delta=7.70-7.63 (m, 2H), 7.59-7.52 (m, 2H). (0338) 7.04 (d, J=8 Hz, 2H), 6.85 (d, J=8.4 Hz, 2H), 5.42 (s, 2H), 5.21 (s, 1H), 5.05 (s, 2H), 2.60 (t, J=7.6 Hz, 2H), 2.07 (s, 3H), 1.60-1.55 (m, 2H), 1.47 (s, 6H), 0.87 (t, J=7.2 Hz, 3H); (0339) Mass: 559 [M+H]+.

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Patent; API CORPORATION; Seki, Masahiko; US2015/239854; (2015); A1;,
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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

61(b) (5-Methyl-2-oxo-1,3-dioxolen-4yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate A mixture of 1.4 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (a) above] and 48 ml of 75% v/v aqueous acetic acid was stirred at 60 C. for 1 hour, after which it was concentrated by evaporation under reduced pressure. The residue was dissolved in toluene, and the resulting solution was concentrated by distillation under reduced pressure; this was repeated a further time in order to remove the remaining water and acetic acid. The residue thus obtained was purified by column chromatography through silica gel using 1:9 and 1:4 by volume mixtures of methanol and methylene chloride as the eluent, to give 0.73 g of the title compound, melting at 170-172 C. Nuclear Magnetic Resonance Spectrum (CDCl3), delta ppm: 0.93 (3H, triplet, J=7.5 Hz); 1.63 (6H, singlet); 1.6-1.8 (2H, multiplet); 2.19 (3H, singlet); 2.70 (2H, triplet, J=7.5 Hz); 5.00 (2H, singlet); 5.45 (2H, singlet); 6.83 (2H, doublet, J=8 Hz); 7.10 (2H, doublet, J=8 Hz); 7.42-7.63 (3H, multiplet); 7.83 (1H, doublet of doublets, J=1 & 7.5 Hz).

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Patent; Sankyo Company, Limited; US5616599; (1997); 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.

78(b) (5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate 75 ml of water were added to a suspension of 29.3 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (a) above] in 225 ml of acetic acid, and the resulting mixture was stirred at 60 C. for 1.5 hours. At the end of this time, 75 ml of water were added to the mixture, which was then cooled. Precipitated trityl alcohol was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure. Toluene was added to the residue, and the mixture was again concentrated by evaporation under reduced pressure, to remove the remaining water and acetic acid. The residue was crystallized in ethyl acetate, to give 16.6 g of the title compound as crystals, melting at 177-180 C. (with decomposition). The Nuclear Magnetic Resonance Spectrum of this compound was identical with that of the compound obtained as described in Example 61(b).

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Patent; Sankyo Company, Limited; US5616599; (1997); A;,
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144690-92-6,In homogeneous catalysis, the catalyst is in the same phase as the reactant. The number of collisions between reactants and catalyst is at a maximum.In a article,Triphenyl methyl olmesartan,introducing its new discovery.

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 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 20 C. 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 20 C. and the layers were separated. The organic layer was dried over sodium sulfate and ethyl acetate was distilled off completely under vacuum at below 45 C. to obtain a residual mass. To the residual mass was added ethyl acetate (400 ml) at 40 C. and then heated to 75 to 80 C. The contents were maintained for 30 minutes at 75 to 80 C. The reaction mass was cooled to room temperature and stirred for 1 hour. The reaction mass was further cooled to 10 to 15 C. and stirred for 1 hour 30 minutes, filtered. The solid obtained was dried at 40 to 45 C. 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%.

The proportionality constant is the rate constant for the particular unimolecular reaction. the reaction rate is directly proportional to the concentration of the reactant. I hope my blog about 144690-92-6 is helpful to your research. 144690-92-6

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Patent; HETERO RESEARCH FOUNDATION; Parthasaradhi Reddy, Bandi; Rathnakar Reddy, Kura; Muralidhara Reddy, Dasari; Raji Reddy, Rapolu; Ramakrishna Reddy, Matta; Vamsi Krishna, Bandi; US2013/190506; (2013); A1;,
1,3-Benzodioxole – Wikipedia
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144690-92-6,In homogeneous catalysis, the catalyst is in the same phase as the reactant. The number of collisions between reactants and catalyst is at a maximum.In a article,Triphenyl methyl olmesartan,introducing its new discovery.

Trityl olmesartan medoxomil (8 g, 10 mmol) is added to a mixture of acetone (35 ml) and water (10 ml). To the resulting suspension 37 % aqueous hydrochloric acid (2.5 ml, 30 mmol) is added. The mixture is then stirred at room temperature for 4 h. Water (130 ml) is added and the mixture is stirred for additional 30 minutes. The precipitated triphenylmethanol is filtered off. The filtrate is concentrated in vacuum at 40 C to 100 ml, and then stirred vigorously for 1 h at room temperature and then additional 30 minutes at 0 C. The precipitate is filtered to give 4.7 g of olmesartan medoxomil hydrochloride Form A (98.3 % area)

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; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
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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.

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%.

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Patent; API Corporation; SEKI, Masahiko; EP2891650; (2015); A1;,
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144690-92-6,is a common compound. C48H44N6O6.In an article, once mentioned the new application about 144690-92-6.

A mixture of trityl olmesartan medoxomil (4.0 g), methanol (20 mL), and water (10 mL) is stirred at 25-35C for 15 minutes. Aqueous HCI (1 mL) is added drop-wise at 25-35C. The mixture is cooled to 0-50C. Water (30 mL) is added and the mixture is further stirred at 0-5C for 1 hour. The insoluble material is removed by filtration and the pH of the filtrate is adjusted to about 3-4 by adding 10% aqueous NaHCOs at 25-35C. The mixture is extracted with dichloromethane (3chi40 ml_). The organic layers are combined and washed with water (40 ml_). The solvent is distilled under reduced pressure below 400C. Ethyl acetate (10 ml_) is added to the residue and the mixture is heated to 50-600C and stirred for 1 hour. The mixture is cooled to 25-35C. The formed solid is filtered, washed with ethyl acetate (5 ml_), and dried under vacuum at 60-700C (yield 2.0 g).

The proportionality constant is the rate constant for the particular unimolecular reaction. the reaction rate is directly proportional to the concentration of the reactant. I hope my blog about 144690-92-6 is helpful to your research. 144690-92-6

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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;,
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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

Trityl olmesartan medoxomil (250 g, 310 mmol) (97.3 % area) is dissolved in THF (1560 ml) and 48 % aqueous hydrobromic acid (70.6 ml, 625 mmol) is added slowly. The mixture is stirred for at 25 C. After 1 hour the precipitate forms. The mixture is stirred for 1 additional hour at 25 C, then cooled to -5 C and stirred for 1.5 hours at -5 C. The precipitate is filtered. 940 ml of THF is added to the precipitate and the mixture is stirred for 1 h at 25 C and then 1 hour at -5 C. Then precipitate is filtered off and washed with cold THF (150 ml). It is then dissolved in a mixture of water (875 ml) and acetone (440 ml). To a clear solution 5 % aqueous solution of NaHCO3 is added to raise pH to 5.15. The mixture is stirred for 1 hour at room temperature and 1 hour at 0 C. The precipitate is filtered, washed with water and then recrystallized from a mixture of acetonitrile (280 ml) and water (70 ml) to give 124.5 g of olmesartan medoxomil (99.68 % area)

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Patent; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
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