HRID652547

反应详情

EQUATION

反应方程式

HRID 652547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 21 g of 2,6-dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,2-dimethyl-1,3-dioxolan-4-yl)methoxyphenyl]ethoxycarbonyl)-1,4-dihydropyridine (6) in 150 mL of acetone and 50 mL of water was treated with 10 mL of hydrochloric acid and the mixture heated at reflux for 6 h. Water (500 mL) was added and the mixture was extracted with ether. The ether layer was dried over Na2SO4 and evaporated to an oil which was purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane) to give 12 g of 2,6-dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,3-dihydroxypropoxy)phenyl]ethoxycarbonyl)-1,4-dihydropyridine (1) as a thick oil which crystallized upon trituration with ethyl acetate, m.p. 117°-118° C.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 6 h
  3. extractionthe mixture was extracted with ether
  4. dry with materialThe ether layer was dried over Na2SO4
  5. customevaporated to an oil which
  6. customwas purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane)