HRID464929

反应详情

EQUATION

反应方程式

HRID 464929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2 g (5 mmole) of 1-[4-chloro-2-benzoylphenyl]-3-phthalimidopropyne and 1/2 teaspoonful of Raney nickel in 25 ml of tetrahydrofuran was hydrogenated at room temperature and atmospheric pressure. When 240 ml of hydrogen was absorbed, the catalyst was separated by filtration and the filtrate concentrated at reduced pressure to dryness. The residue was crystallized from a mixture of ether and petroleum to give crude product as a tan solid, mp 94°-97° C. Recrystallization from ether gave pale yellow prisms, mp 98°-99° C.

WORKUP

后处理

  1. customwas hydrogenated at room temperature
  2. customWhen 240 ml of hydrogen was absorbed
  3. customthe catalyst was separated by filtration
  4. concentrationthe filtrate concentrated at reduced pressure to dryness
  5. customThe residue was crystallized from a mixture of ether and petroleum
  6. customto give crude product as a tan solid, mp 94°-97° C
  7. customRecrystallization from ether
  8. customgave pale yellow prisms, mp 98°-99° C.