HRID265147

反应详情

EQUATION

反应方程式

HRID 265147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.75 ml of a 0.15N solution of sodium ethoxide in ethanol was added to a solution of 1.69 g of ethyl 2-acetoxymethyl-4-(1-hydroxy-1-methylethyl)-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in Example 102(a)] in 15 ml of ethanol, and the mixture was stirred at room temperature for 5 minutes. The reaction solution was then concentrated by evaporation under reduced pressure, ethyl acetate and water were added to the residue, and the ethyl acetate layer was separated. This ethyl acetate layer was washed with an aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate, after which it was concentrated by evaporation under reduced pressure. The resulting residue was purified by recrystallization from a mixture of diethyl ether and diisopropyl ether, to give 1.47 g of the title compound as crystals, melting at 151°-152° C.

WORKUP

后处理

  1. concentrationThe reaction solution was then concentrated by evaporation under reduced pressure, ethyl acetate and water
  2. additionwere added to the residue
  3. customthe ethyl acetate layer was separated
  4. washThis ethyl acetate layer was washed with an aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationafter which it was concentrated by evaporation under reduced pressure
  7. customThe resulting residue was purified by recrystallization from a mixture of diethyl ether and diisopropyl ether