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
To a solution of 2-amino-4′-bromoacetophenone hydrochloride (8.2 g), 4-pentyloxybenzoic acid (6.8 g) and 1-hydroxybenzotriazole (4.42 g) in dichloromethane (80 ml) was added 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide (WSCD) (6.0 ml), and stirred for 3 hours at ambient temperature. The reaction mixture was diluted with dichloromethane (800 ml), and washed with 1N hydrochloric acid, saturated sodium hydrogen carbonate aqueous solution and brine. The organic layer was dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The solids were slurried in ethyl acetate, and collected by filtration to give 2-(4-pentyloxybenzamido)-4′-bromoacetophenone (2.49 g).
WORKUP
后处理
- washwashed with 1N hydrochloric acid, saturated sodium hydrogen carbonate aqueous solution and brine
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationMagnesium sulfate was filtered off
- customthe filtrate was evaporated under reduced pressure
- filtrationcollected by filtration