HRID1358318

反应详情

EQUATION

反应方程式

HRID 1358318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.8 g of 4,6-dichloro-5-(p-tolyl)-pyrimidine and 1.68 g of 4-tert.-butylbenzene sulfonamide potassium salt in 20 ml of DMSO was stirred at room temperature for 24 h. The mixture was poured onto 200 ml of water and extracted twice with 100 ml of diethyl ether. The organic layers was extracted twice with 50 ml of water. The combined aqueous layers was acidified with conc. hydrochloric acid. The resulting fine suspension was extracted twice with ethyl acetate. The combined organic layers was dried over Na2SO4 and evaporated. The residue was dried under high vacuum to give 1.34 g 4-tert.-butyl-N-[6-chloro-5-(p-tolyl)-4-pyrimidinyl]-benzene sulfonamide as a white powder. LC-MS: tR=5.92 min, [M+1]+=416.20, [M−1]−=414.24.

WORKUP

后处理

  1. extractionextracted twice with 100 ml of diethyl ether
  2. extractionThe organic layers was extracted twice with 50 ml of water
  3. extractionThe resulting fine suspension was extracted twice with ethyl acetate
  4. dry with materialThe combined organic layers was dried over Na2SO4
  5. customevaporated
  6. customThe residue was dried under high vacuum