Réaction #339107

ord-edb1e9fb023140cda37768f2d9730a17

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated
  2. 2
    Températureto reflux for 3 hours
  3. 3
    Températureto cool to around room temperature
  4. 4
    Extractionthe mixture was extracted with ethyl acetate three times
  5. 5
    ConcentrationThe resulting organic layer was concentrated under reduced pressure
  6. 6
    Lavagethe residue was washed with toluene

Mode opératoire

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:

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07867949B2uspto-grants-2011_01