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144690-92-6, 21.6 g of triethylolmethane-containing methoxycinnamic acid (formula 1a), 3 g of hydroxylamine hydrochloride, 14 mL of acetone and 70 mL of ethanol were added to the reaction part, followed by stirring at 25 to 40 C for 4 hours. When the reaction was completed, the reaction solution was concentrated under reduced pressure. Ethyl acetate (80 mL) was added to the residue, and the mixture was stirred for 3 hours to precipitate crystals. The precipitated crystals were stirred at 20 to 25 C for 2 hours, filtered and washed with 20 mL of purified water. To the filtrate was added 40 mL of ethyl acetate, the temperature was cooled to 0 to 5 C, The pH of the filtrate was adjusted to pH 5.0 to 6.0 by adding 45 g of triethylamine to the filtrate, and crystals were slowly precipitated. The precipitated crystals were stirred at 0 to 5 C for 3 hours, filtered, washed with 30 mL of purified water and 30 mL of acetone, and dried under reduced pressure for 15 hours to obtain 12.3 g (yield 82%, purity 99.96%) of olmesartan methoxysilane (Formula 1b).
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Reference£º
Patent; DONGBANG FTL CO., LTD; Song, Tae Hong; Jung, Hun Suk; Jang, Do Yeon; Moon, Chung Sun; Jung, Hee Jung; (18 pag.)KR101526249; (2015); B1;,
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