HRID2235498

反应详情

EQUATION

反应方程式

HRID 2235498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 0.60 g (3.0 mmol) of (3-nitrophenyl)thiourea in 25 mL of carbon tetrachloride was added 0.17 mL (3.4 mmol) of bromine in 10 mL of carbon tetrachloride dropwise over 1 h. The mixture was heated to reflux for 18 h, cooled to room temperature and the precipitate that formed was collected by filtration. The precipitate was slurried in glacial acetic acid and the solids were collected by filtration. The solids thus obtained were slurried in water and saturated potassium carbonate was added until the pH was about 9. The free base was collected by filtration to give 0.30 g (51%) of the title compound as a light orange solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 18 h
  3. customthe precipitate that formed
  4. filtrationwas collected by filtration
  5. filtrationthe solids were collected by filtration
  6. customThe solids thus obtained
  7. filtrationThe free base was collected by filtration