反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 dichloromethane (70 ml) was added to triflic anhydride (16.75 g) in dichloro methane (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 dichloromethane (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 dichloromethane, 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
- waitto stand at room temperature for 4 days
- concentrationconcentrated
- temperatureheated on a steam bath with 10% sodium hydroxide (250 ml)
- additiondiluted with 300 ml of water
- extractionextracted with dichloromethane
- customdried
- filtrationfiltered
- concentrationconcentrated
- customto give an oil