Reaktion #310047

Reaktionsgleichung

2-fluoro-3-methyl-nitrobenzene

tert-butoxycarbonylhydrazine

→

product

Ausbeute 80.0%

tert-butyl N-(2-methyl-6-nitro-phenyl)-hydrazino-carboxylate

Ausbeute 80.0%

Lösungsmittel

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheating
2. 2
   Extraktionextracted with ethyl acetate several times
3. 3
   SonstigeThe organic phases are collected
4. 4
   Sonstigedried on magnesium sulfate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated under reduced pressure
7. 7
   Sonstigeis purified by chromatography on silica gel (cyclohexane/ethyl acetate: 80/20)

Vorschrift

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.

Quelle