HRID394898

反应详情

EQUATION

反应方程式

HRID 394898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4,4,4-trifluoro-1-(3-fluoro-4-(1,3-thiazol-4-yl)phenyl)-1,3-butanedione (503 mg, 1.59 mmol) and 5-hydrazino-2-pyridinesulfonamide hydrochloride (392 mg, 1.74 mmol) in ethanol (22 ml) was stirred at reflux for 28 h. After cooling, the solvent was removed and the residue was added water, extracted with ethyl acetate. The extracts was dried (MgSO4) and concentrated. This was purified on silica gel eluting with ethyl acetate/hexane (1:4/1:3/1:2) to afford 172 mg (23.0%) of the titled compound as a yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 28 h
  2. temperatureAfter cooling
  3. customthe solvent was removed
  4. additionthe residue was added water
  5. extractionextracted with ethyl acetate
  6. dry with materialThe extracts was dried (MgSO4)
  7. concentrationconcentrated
  8. customThis was purified on silica gel eluting with ethyl acetate/hexane (1:4/1:3/1:2)