Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1.C(O)C.C(O[CH:27](OCC)[N:28]([CH3:30])[CH3:29])C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[C:9](=[CH:27][N:28]([CH3:30])[CH3:29])[N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 130 °C
Versuchsvorschrift
A suspension of 50 gm of 7-chloro-5-(2'-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 100 ml of N,N-dimethyl-formamide diethylacetal was heated to 130°C in a vessel equipped with a descending condenser, whereby a clear solution was formed after a short time. The temperature of the reaction solution was maintained at 130°C for 40 minutes, during which time the ethanol formed by the reaction slowly distilled over. Thereafter, the reaction solution was allowed to cool, and the red precipitate was collected by vacuum filtration, washed with petroleum ether and recrystallized from methanol, whereupon it had a melting point of 239°-241°C. It was identified to be the compound of the formula ##SPC6##
Aufarbeitung
- customequipped with a descending condenser
- customwhereby a clear solution was formed after a short time
- customformed by the reaction
- distillationslowly distilled over
- temperatureto cool
- filtrationthe red precipitate was collected by vacuum filtration
- washwashed with petroleum ether
- customrecrystallized from methanol, whereupon it
Quellen und Nachweise
- ORD-Eintrag
- ord-7f87dbed62cc469cb7913123ec3770ae
- Quelldatensatz
- uspto-grants-1976_05
- Patentnummer
- US03956492
Verknüpfte Notizen
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