HRID1198426

反应详情

EQUATION

反应方程式

HRID 1198426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.62 g (4.0 mmole) 3-[5-(bromomethyl)-4-chloro-2-fluorophenyl]-4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazole, 0.44 mL ethyl mercaptoacetate and 0.55 g K2CO3 was slurried in 25 mL of acetone. The reaction mixture was allowed to stir at room temperature overnight. After dilution with 100 mL of cold water, the mixture was extracted with ethyl acetate, the organic extracts washed with water, dried with MgSO4 and concentrated in vacuo. The residue was purified by chromatography to afford 1.7 g (96%) of (((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methyl)thio)acetic acid, ethyl ester as a white solid; mp 63° C.

WORKUP

后处理

  1. extractionAfter dilution with 100 mL of cold water, the mixture was extracted with ethyl acetate
  2. washthe organic extracts washed with water
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography