Reaktion #2374050

Reaktionsgleichung

5-Amino-N-(1-hydroxy-2,2,2-trichloroethyl)salicylamide

sulphuric acid

→

6-amino-3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazin-4-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONpoured onto ice (1 l.)
2. 2
   Filtrationfiltered
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   Filtrationthe precipitated product was filtered off
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried at 60° C.

Vorschrift

5-Amino-N-(1-hydroxy-2,2,2-trichloroethyl)salicylamide (23.0 g.) and concentrated sulphuric acid (115 ml.) were heated on a steam bath for 1 hour, then poured onto ice (1 l.). The resulting mixture was stirred for 30 minutes and filtered. The filtrate was adjusted to pH 5 with 5 N sodium hydroxide solution and stirred for 30 minutes, and the precipitated product was filtered off, washed with water, and dried at 60° C. to give 6-amino-3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazin-4-one, m.p. 172°-174° C.

Quelle