反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
2.49 g (0.01 mol) of 1-[p-(2-methoxycarbonylaminovinyl)-phenoxy]-2,3-epoxy-propane are dissolved in 25 ml of acetonitrile and added dropwise to a boiling stirred solution of 1.42 g (0.0095 mol) of 3-amino-1-phenylbutane in 20 ml of acetonitrile. The mixture is stirred for 20 hours under reflux, the solvent is removed by distillation under reduced pressure and the oil which remains is partitioned between 120 ml of 0.1 N hydrochloric acid and 100 ml of ethyl acetate. The hydrochloric acid extract is separated off, rendered alkaline with sodium carbonate and extracted four times with 50 ml of ethyl acetate at a time. The organic phases are dried over sodium sulphate and evaporated in vacuo. The resulting oil yields 1-[p-(2-methoxycarbonylaminovinyl)-phenoxy]-2-hydroxy-3-(1-methyl-3-phenyl-propyl)-amino propane of melting point 126°-127° C., from ethyl acetate.
WORKUP
后处理
- additionadded dropwise to a boiling
- temperatureunder reflux
- customthe solvent is removed by distillation under reduced pressure
- customthe oil which remains is partitioned between 120 ml of 0.1 N hydrochloric acid and 100 ml of ethyl acetate
- extractionThe hydrochloric acid extract
- customis separated off
- extractionextracted four times with 50 ml of ethyl acetate at a time
- dry with materialThe organic phases are dried over sodium sulphate
- customevaporated in vacuo