HRID2091616

反应详情

EQUATION

反应方程式

HRID 2091616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromothiazole-2-carboxylic acid (2.0 g, 9.8 mmol) in methanol (10 mL) was added thionyl chloride (710 μL, 9.8 mmol) and the mixture was refluxed for 3 hours. The solvent was removed under reduced pressure, and the residue was suspended in ethanol (10 mL). To this suspension was added hydrazine hydrate (2.4 mL, 49 mmol), and the reaction was heated to reflux for 90 minutes. The solvent was removed under reduced pressure, and the residue suspended in acetonitrile, filtered, and the solids were washed with acetonitrile, diethyl ether, and dried under vacuum to afford 1.7 g (77%) of 4-bromothiazole-2-carbohydrazide as a yellow solid. M+1=222.1

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 3 hours
  2. customThe solvent was removed under reduced pressure
  3. temperaturethe reaction was heated
  4. temperatureto reflux for 90 minutes
  5. customThe solvent was removed under reduced pressure
  6. filtrationfiltered
  7. washthe solids were washed with acetonitrile, diethyl ether
  8. customdried under vacuum