HRID1250415

反应详情

EQUATION

反应方程式

HRID 1250415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 16.4 g (0.2 mol) of 3-aminocrotononitrile in 100 cm3 of n-pentanol were added 26.9 g (0.22 mol) of benzylhydrazine and the mixture was then heated at reflux for 12 hours. The n-pentanol was subsequently distilled off under reduced pressure and a thick oil was obtained, which was purified by chromatography on silica gel. A pale yellow solid was obtained, which was crystallized from isopropyl ether and was then filtered on a sinter funnel. After drying under vacuum at 40° C., 17 g of the expected product were obtained in the form of a pale yellow solid, the melting point of which was from 76 to 78° C.

WORKUP

后处理

  1. temperaturethe mixture was then heated
  2. temperatureat reflux for 12 hours
  3. distillationThe n-pentanol was subsequently distilled off under reduced pressure
  4. customa thick oil was obtained
  5. customwhich was purified by chromatography on silica gel
  6. customA pale yellow solid was obtained
  7. customwhich was crystallized from isopropyl ether
  8. filtrationwas then filtered on a sinter funnel
  9. customAfter drying under vacuum at 40° C.