HRID222865

反应详情

EQUATION

反应方程式

HRID 222865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureheating
  2. extractionextracted with ethyl acetate several times
  3. customThe organic phases are collected
  4. customdried on magnesium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customis purified by chromatography on silica gel (cyclohexane/ethyl acetate: 80/20)