Reaktion #2374037

Reaktionsgleichung

3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carbonyl chloride

n-propylamine

→

3,4-dihydro-4-oxo-N-propyl-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carboxamide

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Sonstigethe solvent was evaporated under reduced pressure
3. 3
   Sonstigeto give a sticky solid residue
4. 4
   SonstigeThe residue was triturated with water
5. 5
   workup.STIRRINGthe resulting suspension was stirred for 30 minutes
6. 6
   Filtrationfiltered
7. 7
   WaschenThe solid product was washed with water
8. 8
   Sonstigedried
9. 9
   Sonstigecrystallised from ethanol

Vorschrift

Powdered 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carbonyl chloride (5.0 g.) was stirred while a solution of n-propylamine (5 ml) in methanol (100 ml.) was added, the resulting solution was stirred for 30 minutes, and the solvent was evaporated under reduced pressure to give a sticky solid residue. The residue was triturated with water and the resulting suspension was stirred for 30 minutes and filtered. The solid product was washed with water, dried and crystallised from ethanol to give 3,4-dihydro-4-oxo-N-propyl-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carboxamide, m.p. 228°-230° C.

Quelle