Diethylamine → 4-dichloromethylene-N,N-diethyl-2-trichloromethylbenzo[1,3]dioxin-6-carboxamide
Reaktionsgleichung
[Cl:1][C:2]([Cl:21])([Cl:20])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17](Cl)=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.[CH2:22]([NH:24][CH2:25][CH3:26])[CH3:23]>>[Cl:10][C:9]([Cl:11])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([N:24]([CH2:25][CH3:26])[CH2:22][CH3:23])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:20])([Cl:21])[Cl:1])[O:8]1Komponenten
3
Versuchsvorschrift
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.
Aufarbeitung
- temperaturewas heated
- temperatureunder reflux for 2 hrs