Reaktion #2374036

Reaktionsgleichung

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

→

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

Lösungsmittel

n-butanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated on a steam bath for 30 minutes
2. 2
   Sonstigethe solvent was evaporated under reduced pressure
3. 3
   SonstigeThe sticky solid residue was triturated with petroleum ether (b.p. 60°-80° C.)
4. 4
   Filtrationfiltered
5. 5
   Waschenwashed with petroleum ether
6. 6
   Sonstigecrystallised from n-butanol

Vorschrift

A suspension of powdered 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carbonyl chloride (5.0 g.) in n-butanol (100 ml.) was heated on a steam bath for 30 minutes. The solution was cooled to ambient temperature, and the solvent was evaporated under reduced pressure. The sticky solid residue was triturated with petroleum ether (b.p. 60°-80° C.), filtered, washed with petroleum ether and crystallised from n-butanol to give butyl 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carboxylate, m.p. 134°-136° C.

Quelle