Reaktion #2374049

Reaktionsgleichung

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

thionyl chloride

→

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

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 1 hour
2. 2
   Sonstigethe white suspension so formed
3. 3
   Filtrationwas filtered off
4. 4
   Waschenwashed with water
5. 5
   Sonstigedried at 60° C.
6. 6
   Extraktionextracted with toluene (3×200 ml.)
7. 7
   Sonstigethe solvent was evaporated

Vorschrift

3,4-Dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carboxamide (prepared as described in Example 10--1.0 g.) and thionyl chloride (20 ml.) were heated together under reflux for 1 hour, cooled to room temperature, and drowned into ice-water (200 ml.). After stirring for 1 hour, the white suspension so formed was filtered off, washed with water, dried at 60° C. and extracted with toluene (3×200 ml.). The toluene extracts were combined, and the solvent was evaporated to give 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carbonitrile, m.p. 212°-214° C.

Quelle