HRID274587

反应详情

EQUATION

反应方程式

HRID 274587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-4'-methylbenzophenone (10 g), 3,3-dimethoxypropionitrile (10.9 g), p-toluenesulfonic acid. monohydrate (1.0 g) in toluene (120 ml) was heated under reflux for 4 hours. After addition of water, the reaction mixture was extracted with ethyl acetate and the extract was concentrated to dryness. The residue was purified by column chromatography on silica gel. Recrystallization from isopropyl ether afforded pale yellow prisms (5.67 g, 49%), m.p. 96°-97° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. concentrationthe extract was concentrated to dryness
  5. customThe residue was purified by column chromatography on silica gel
  6. customRecrystallization from isopropyl ether afforded pale yellow prisms (5.67 g, 49%), m.p. 96°-97° C.