HRID965624

反应详情

EQUATION

反应方程式

HRID 965624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4,6-dichloro-5-p-tolyl-pyrimidine (2.0 g) disolved in DMSO (35 ml) was added di-isopropyl-ethyl-amine (1.46 ml) followed by 2-phenyl-ethenesulfonamide potassium salt (2.78 g). The mixture was stirred for 48 h at rt then poured onto water (500 ml) and diethylether (250 ml) was added and the solution was stirred for 30 minutes. The layers were separated and the water layer was acidified with acetic acid (2.0 ml) and cooled to 0° C. for 1 h. The precipitated product was filtered off and washed with water and diethylether and dried to give 2-phenyl-ethenesulfonic acid(6-chloro-5-p-tolyl-pyrimidin-4-yl)-amide (2.02 g). tR=5.32 (LC); M+=386.23 (ES+); M−=384.22 (ES−).

WORKUP

后处理

  1. additionwas added
  2. stirringthe solution was stirred for 30 minutes
  3. customThe layers were separated
  4. temperaturecooled to 0° C. for 1 h
  5. filtrationThe precipitated product was filtered off
  6. washwashed with water and diethylether
  7. customdried