Reaktion #2374051

Reaktionsgleichung

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

sulphuric acid

sodium chloride

→

3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-sulphonic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated on a steam bath for 18 hours
2. 2
   Extraktionextracted with ethyl acetae (4×100 ml.) The extracts
3. 3
   Sonstigedried
4. 4
   Sonstigethe solvent was evaporated
5. 5
   Sonstigethe residue was crystallised from glacial acetic acid

Vorschrift

A mixture of 3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazin-4-one (10 g.--obtained as described in Example 3) and concentrated sulphuric acid (100 ml.) was heated on a steam bath for 18 hours, and drowned into ice (400 g.). The resulting solution was saturated with sodium chloride and extracted with ethyl acetae (4×100 ml.) The extracts were combined and dried, the solvent was evaporated, and the residue was crystallised from glacial acetic acid to give 3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-sulphonic acid, m.p. > 260° C.

Quelle