HRID2074033

反应详情

EQUATION

反应方程式

HRID 2074033 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 in 150 mL of acetone and 50 mL of water is treated with 10 mL of hydrochloric acid and the mixture heated at reflux for 6 h. Water (500 mL) is added and the mixture was extracted with ether. The ether layer is dried over Na2SO4 and evaporated to an oil which is purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane) to give 2,6-dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,3-dihydroxypropoxy)phenyl]ethoxycarbonyl)-1,4-dihydropyridine, m.p. 117-118° C., [α]D =-33.5°.

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 is dried over Na2SO4
  5. customevaporated to an oil which
  6. customis purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane)