HRID22647

反应详情

EQUATION

反应方程式

HRID 22647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.32 g (7.7 mmol) methyl-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-amine and 1.50 g (11.6 mmol) N-ethyldiisopropylamine in 20 ml tetrahydrofuran was cooled in an ice bath and 2.72 g (8.5 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride were added dropwise. The reaction mixture was stirred at room temperature overnight and evaporated in vacuo. The residue was suspended in 200 ml 1 N sodium carbonate solution and extracted three times with 200-ml portions of ethyl acetate. The combined organic layers were dried (sodium sulfate) and evaporated. The residue was crystallized from ethanol to give 3.60 g (80%) of the title compound as white crystals.

WORKUP

后处理

  1. customevaporated in vacuo
  2. extractionextracted three times with 200-ml portions of ethyl acetate
  3. dry with materialThe combined organic layers were dried (sodium sulfate)
  4. customevaporated
  5. customThe residue was crystallized from ethanol