HRID1088210

反应详情

EQUATION

反应方程式

HRID 1088210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.6 g (0.05 mol) of 3-bromoaniline in 100 ml of dimethylformamide is added dropwise to a solution of 12.0 g (0.06 mol) of 2,4-dichloro-5-nitrothiazole in 100 ml of dimethylformamide at 0° C. to 5° C. in the course of about 2 hours and the mixture is subsequently stirred at the same temperature for a further 4 hours. It is then stirred into 1,000 ml of ice-water and the precipitate is filtered off, washed with water and dried. To remove excess 2,4-dichloro-5-nitrothiazole, the product is stirred in 80 ml of petroleum ether at room temperature, filtered off, washed with petroleum ether and dried. 16.0 g (95.7% of theory) of 2-(3-bromophenylamino)-4-chloro-5-nitrothiazole of melting point 191° C. to 192° C. (decomposition) are thus obtained.

WORKUP

后处理

  1. filtrationthe precipitate is filtered off
  2. washwashed with water
  3. customdried
  4. customTo remove excess 2,4-dichloro-5-nitrothiazole
  5. stirringthe product is stirred in 80 ml of petroleum ether at room temperature
  6. filtrationfiltered off
  7. washwashed with petroleum ether
  8. customdried