HRID34663

反应详情

EQUATION

反应方程式

HRID 34663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6.78 g (21.12 mmol) of 6-bromo-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-one, hydrobromide and 1.93 g (25.35 mmol) of thiourea in 100 ml of water is heated on a steam bath for 2 hours. The mixture is filtered hot through a pad of Celite to remove a small amount of insoluble solid. The filtrate is cooled, basified with ammonium hydroxide, and a precipitate is collected. Recrystallization from acetonitrile affords 4.26 g (92.8%) of the title compound as a tan solid; mp 220°-222° C. (dec.).

WORKUP

后处理

  1. filtrationThe mixture is filtered hot through a pad of Celite
  2. customto remove a small amount of insoluble solid
  3. temperatureThe filtrate is cooled
  4. customa precipitate is collected
  5. customRecrystallization from acetonitrile