HRID36989

反应详情

EQUATION

反应方程式

HRID 36989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

A mixture of 2-(1-adamantyl)ethanol (10.7 g and diisopropylethylamine (11 ml) in methylene chloride (70 ml) was added to triflic anhydride (16.75 g) in methylene chloride (70 ml) at -78° C. under argon. After stirring the mixture at -78° C. for 45 minutes, 1-acetyl-2-n-butyl-5 -(acetoxymethyl)imidazole in methylene chloride (50 ml) was added and the mixture was allowed to stand at room temperature for 4 days, then concentrated and heated on a steam bath with 10% sodium hydroxide (250 ml), diluted with 300 ml of water, extracted with methylene chloride, dried, filtered and concentrated to give an oil. Chromatography (silica gel) in methanol-chloroform gives 5-acetoxymethyl-1-[2-(1-adamantyl)ethyl]-2-n-butylimidazole.

WORKUP

后处理

  1. waitto stand at room temperature for 4 days
  2. concentrationconcentrated
  3. temperatureheated on a steam bath with 10% sodium hydroxide (250 ml)
  4. additiondiluted with 300 ml of water
  5. extractionextracted with methylene chloride
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give an oil