HRID2247326

反应详情

EQUATION

反应方程式

HRID 2247326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl isocyanate (0.015 ml, 0.19 mmol) is added to a stirred solution of 4-(2-amino-4-methyl-thiazol-5-yl)-2,6-dichloro-benzenesulfonamide (Example 26) (0.043 g, 0.127 mmol) in dry dimethylformamide (1.0 ml) under argon. After heating at 85° C. for 3 hours more ethyl isocyanate (0.015 ml, 0.19 mmol) is added and heating continued for a further hour. The reaction is concentrated in vacuo and the product is purified by chromatography on silica eluting with ethyl acetate—hexane (1:1 increasing to 4:1) to give the title compound. MH+ (TOF, MS, ES+): 408.9, 410.9, 412.8

WORKUP

后处理

  1. additionis added
  2. temperatureheating
  3. waitcontinued for a further hour
  4. concentrationThe reaction is concentrated in vacuo
  5. customthe product is purified by chromatography on silica eluting with ethyl acetate—hexane (1:1 increasing to 4:1)