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
PROCEDURE
实验过程
83.3 Grams (0.324 mole) of 2-tert-butyl-3-(4-chlorophenyl)-3-hydroxypropionic acid and 125 g (0.77 mole) of 1,1'-carbonyldiimidazole were mixed with 700 ml of tetrahydrofuran, and the mixture was heated under reflux for 3 hours with stirring. After concentrating the reaction solution under reduced pressure, water and then diethyl ether were added to the residue which was then washed with water. The ether layer was separated and concentrated to form crystals with a small amount of ether left in the system. The crystal was filtered off and washed with a small amount of ether to obtain 50.6 g (38.5%) of N-{2-tert-butyl-3-(4-chlorophenyl)-3-(1-imidazolylcarbonyloxy)propanoyl}-imidazole. m.p., 69°-71° C.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- concentrationAfter concentrating the reaction solution under reduced pressure, water
- additiondiethyl ether were added to the residue which
- washwas then washed with water
- customThe ether layer was separated
- concentrationconcentrated
- customto form crystals with a small amount of ether
- waitleft in the system
- filtrationThe crystal was filtered off
- washwashed with a small amount of ether