HRID921278

反应详情

EQUATION

反应方程式

HRID 921278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 4-amino-dimethylphenylphosphine oxide (3.7 g, 2.2 mmol) in 15 mL of N,N-Dimethylacetamide and 3.6 mL of Diisopropylethylamine, was allowed to stirred at room temperature for 15 minutes until a clear solution was obtained. 2,4-Dichloro-5-(trifluoromethyl)pyrimidine (5.7 g, 2.6 mmol) was added in four portions over 5 minutes. The reaction mixture was stirred at 60 degrees for 1 hour. The reaction mixture was cooled to room temperature and filtered to obtain a white solid. The white solid was washed with 50 mL of water three times and followed by 50 mL of Ethyl ether three times. The white solid was dried under vacuum to yield desired product (3.8 g, 49% yield). MS ES+: m/z=350.

WORKUP

后处理

  1. customwas obtained
  2. stirringThe reaction mixture was stirred at 60 degrees for 1 hour
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationfiltered
  5. customto obtain a white solid
  6. washThe white solid was washed with 50 mL of water three times
  7. customThe white solid was dried under vacuum