Ammonia methanol → HCID 178421536, Verbindung
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:19])=[C:6]([C:8]2([CH3:18])[C:14]([F:16])([F:15])[CH2:13][O:12][CH2:11][C:10](=S)[NH:9]2)[CH:7]=1.[NH3:20].CO>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:19])=[C:6]([C:8]2([CH3:18])[C:14]([F:16])([F:15])[CH2:13][O:12][CH2:11][C:10](=[NH:20])[NH:9]2)[CH:7]=1Komponenten
3
Versuchsvorschrift
A mixture of 5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepane-3-thione (1.0 g, 2.83 mmol) and 10% NH3/MeOH (25 mL) was stirred in a sealed tube at it for 24 h. Reaction mixture was concentrated and purified by column chromatography on silica gel with 5% MeOH, 2% NH3 in chloroform to furnish the title compound as a pale brown gum. Yield=1.1 g ( ). LCMS: RtH8=0.146 [M+H]+=337.0, 339.0,
Aufarbeitung
- customReaction mixture
- concentrationwas concentrated
- custompurified by column chromatography on silica gel with 5% MeOH, 2% NH3 in chloroform