Reaktion #339107

Reaktionsgleichung

6-chloro-8-methyl-1H-benzo[d]-1,3-oxazine-2,4-dione

methyl carbazate

methanol

→

N-(2-amino-5-chloro-3-methylbenzoyl)-N′-methoxycarbonylhydrazine

Ausbeute 60.2%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturto reflux for 3 hours
3. 3
   Temperaturto cool to around room temperature
4. 4
   Extraktionthe mixture was extracted with ethyl acetate three times
5. 5
   EinengenThe resulting organic layer was concentrated under reduced pressure
6. 6
   Waschenthe residue was washed with toluene

Vorschrift

A mixture of 1.05 g of 6-chloro-8-methyl-1H-benzo[d]-1,3-oxazine-2,4-dione, 0.46 g of methyl carbazate and 20 ml of methanol was heated to reflux for 3 hours. After the reaction mixture was allowed to cool to around room temperature, water was poured thereto and the mixture was extracted with ethyl acetate three times. The resulting organic layer was concentrated under reduced pressure, and the residue was washed with toluene to obtain 0.77 g of N-(2-amino-5-chloro-3-methylbenzoyl)-N′-methoxycarbonylhydrazine of the formula:

Quelle