HRID1358348

反应详情

EQUATION

反应方程式

HRID 1358348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.0 g of 4,6-dichloro-5-(o-methoxyphenoxy)-2-methyl-pyrimidine in 20 ml of DMSO was added 1.76 g of 4-tert.-butyl-benzene sulfonamide potassium salt. The mixture was stirred for 72 h at room temperature. The solution was diluted with 250 ml of water and extracted twice with 200 ml of diehtyl ether. The organic layers were extracted twice with water. The combined aqueous layers were acidified to pH 4 with 5 ml of acetic acid and cooled to 0° C. The precipitated product was filtered off and dried in vacuo to give 1.05 g of 4-tert.-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-methyl-4-pyrimidinyl]-benzene sulfonamide as a pale beige powder. LC-MS: tR=5.64 min, [M+1]+=462.51, [M−1]−=460.63.

WORKUP

后处理

  1. extractionextracted twice with 200 ml of diehtyl ether
  2. extractionThe organic layers were extracted twice with water
  3. temperaturecooled to 0° C
  4. filtrationThe precipitated product was filtered off
  5. customdried in vacuo