HRID554620

反应详情

EQUATION

反应方程式

HRID 554620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To (2-bromo-5-trifluoromethyl-benzyl)-ethyl-amine (22.3 g, 79.1 mmol) and triethylamine (16.53 mL, 118.6 mmol) in CH2Cl2 (200 mL) was added cyclopropanecarbonyl chloride (8.68 mL, 94.9 mmol) dropwise over 15 minutes, and the reaction was stirred at room temperature for 2 hours. The mixture was partitioned between CH2Cl2 and H2O, and the aqueous layer was separated and extracted twice with CH2Cl2. The combined organic layers were dried and concentrated, and the residue was purified by silica gel chromatography (10-30% EtOAc in hexanes) to give cyclopropanecarboxylic acid (2-bromo-5-trifluoromethyl-benzyl)-ethyl-amide.

WORKUP

后处理

  1. customThe mixture was partitioned between CH2Cl2 and H2O
  2. customthe aqueous layer was separated
  3. extractionextracted twice with CH2Cl2
  4. customThe combined organic layers were dried
  5. concentrationconcentrated
  6. customthe residue was purified by silica gel chromatography (10-30% EtOAc in hexanes)