HRID222865
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 250 mg of 2-fluoro-3-methyl-nitrobenzene in 5 mL of DMSO are added 1.065 g of commercial tert-butoxycarbonylhydrazine (5 equivalents). The whole is brought to 100° C. for 10 min under microwave heating. The medium is hydrolyzed and then extracted with ethyl acetate several times. The organic phases are collected, dried on magnesium sulfate, filtered and evaporated under reduced pressure leading to a residue which is purified by chromatography on silica gel (cyclohexane/ethyl acetate: 80/20). 342 mg of product corresponding to the expected product are obtained.
WORKUP
后处理
- temperatureheating
- extractionextracted with ethyl acetate several times
- customThe organic phases are collected
- customdried on magnesium sulfate
- filtrationfiltered
- customevaporated under reduced pressure
- customis purified by chromatography on silica gel (cyclohexane/ethyl acetate: 80/20)