HRID706677

反应详情

EQUATION

反应方程式

HRID 706677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of dimethylamine (2.91 mL, 5.82 mmol, 2.0M THF), NEt3 (0.885 mL, 6.35 mmol) and CH2Cl2 30 mL was cooled to 0° C. 3-(Chloromethyl)benzoyl chloride (1.0 g, 5.29 mmol) was added as a CH2Cl2 solution (3 mL) and the solution was stirred at 0° C. for 2 hours and then at ambient temperature for 2 hours. The reaction was washed with 1N HCl followed by brine, and the organic layer was dried over Na2SO4, filtered and concentrated. The product was purified by column chromatography (EtOAc) to provide 0.745 g (71%) of the product as colorless oil.

WORKUP

后处理

  1. waitat ambient temperature for 2 hours
  2. washThe reaction was washed with 1N HCl
  3. dry with materialthe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe product was purified by column chromatography (EtOAc)