HRID1703099
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
A mixture of 14.5 g. of ethyl p-aminobenzoate, 10 g. of 1-bromo-3-(o-methoxyphenyl)propane and 50 ml. of hexamethylphosphoramide is heated at 130° C. for 15 hours, cooled and diluted with 20 ml. of water. The mixture is chilled, diluted with 50 ml. of cold ethanol:H2O (1:1) and filtered. The solid is washed with three 50 ml. portions of cold ethanol-water (1:1) and with water to give crystals, m.p. 106°-109° C. Recrystallization from ethanol (100 ml.) gives yellow crystals, m.p. 111°-113° C.
WORKUP
后处理
- additionA mixture of 14.5 g
- temperaturecooled
- additiondiluted with 20 ml
- temperatureThe mixture is chilled
- additiondiluted with 50 ml
- filtrationof cold ethanol:H2O (1:1) and filtered
- washThe solid is washed with three 50 ml
- customportions of cold ethanol-water (1:1) and with water to give crystals, m.p. 106°-109° C
- customRecrystallization from ethanol (100 ml.)
- customgives yellow crystals, m.p. 111°-113° C.