HRID2412926

反应详情

EQUATION

反应方程式

HRID 2412926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A reaction mixture was prepared from 13.5 g. of methyl 1-methyl-3-(3-bromophenyl)pyrazole-5-carboxylate and 6.2 g. of sulfuryl chloride in benzene solution. The reaction mixture was heated to refluxing temperature for about 36 hours, and was then cooled and poured into water. The aqueous mixture was extracted with ethyl acetate, and the ethyl acetate extract separated and dried. Removal of the ethyl acetate in vacuo yielded, as a residue, methyl 1-methyl-3-(3-bromophenyl)-4-chloropyrazole-5-carboxylate formed in the above reaction. Recrystallization of the residue from hexane yielded crystalline material melting at 91°-3° C.

WORKUP

后处理

  1. customA reaction mixture was prepared from 13.5 g
  2. temperatureThe reaction mixture was heated
  3. temperatureto refluxing temperature for about 36 hours
  4. temperaturewas then cooled
  5. extractionThe aqueous mixture was extracted with ethyl acetate
  6. extractionthe ethyl acetate extract
  7. customseparated
  8. customdried
  9. customRemoval of the ethyl acetate in vacuo
  10. customyielded, as a residue