Reaktion #311573

Reaktionsgleichung

2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carbonyl chloride

diethylamine

→

4-dichloromethylene-N,N-diethyl-2-trichloromethylbenzo[1,3]dioxin-6-carboxamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 2 hrs
3. 3
   Temperatur, cooled
4. 4
   Filtrationfiltered
5. 5
   Sonstigeto remove diethylamine hydrochloride
6. 6
   SonstigeThe filtrate was evaporated to dryness under reduced pressure
7. 7
   Sonstigethe residue was crystallised from ethanol

Vorschrift

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carbonyl chloride (2 g.) and diethylamine (25 ml.) was heated under reflux for 2 hrs., cooled, and filtered to remove diethylamine hydrochloride. The filtrate was evaporated to dryness under reduced pressure, and the residue was crystallised from ethanol to give 4-dichloromethylene-N,N-diethyl-2-trichloromethylbenzo[1,3]dioxin-6-carboxamide, m.p. 123°-124° C.

Quelle