HRID1703099

反应详情

EQUATION

反应方程式

HRID 1703099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionA mixture of 14.5 g
  2. temperaturecooled
  3. additiondiluted with 20 ml
  4. temperatureThe mixture is chilled
  5. additiondiluted with 50 ml
  6. filtrationof cold ethanol:H2O (1:1) and filtered
  7. washThe solid is washed with three 50 ml
  8. customportions of cold ethanol-water (1:1) and with water to give crystals, m.p. 106°-109° C
  9. customRecrystallization from ethanol (100 ml.)
  10. customgives yellow crystals, m.p. 111°-113° C.