HRID1423334
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 3 hours
- customThe solvent was removed under reduced pressure
- temperaturethe reaction was heated
- temperatureto reflux for 90 minutes
- customThe solvent was removed under reduced pressure
- filtrationfiltered
- washthe solids were washed with acetonitrile, diethyl ether
- customdried under vacuum