Water → methyl (+/-)-(cis)-(7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamate
Reaktionsgleichung
B.[Br:2][C:3]1[C:28]([F:29])=[CH:27][C:6]2[O:7][C:8]3[CH:25]=[C:24]([F:26])[CH:23]=[CH:22][C:9]=3[C@H:10]3[C@H:15]([NH:16][C:17](=[O:20])[O:18][CH3:19])[CH2:14][CH2:13][C:12](=O)[N:11]3[C:5]=2[CH:4]=1.O>C1COCC1.C(OCC)(=O)C>[Br:2][C:3]1[C:28]([F:29])=[CH:27][C:6]2[O:7][C:8]3[CH:25]=[C:24]([F:26])[CH:23]=[CH:22][C:9]=3[C@H:10]3[C@H:15]([NH:16][C:17](=[O:20])[O:18][CH3:19])[CH2:14][CH2:13][CH2:12][N:11]3[C:5]=2[CH:4]=1Komponenten
6
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 30 °C
Versuchsvorschrift
Borane (1.0 M in THF, 38.3 mL, 38.3 mmol) was added dropwise to a stirred solution of methyl (±)-(cis)-(7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-4-oxo-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamate (38.2 mmol) in THF (200 mL). The resulting mixture was stirred at 30° C. for 1 h. Subsequently, water was added dropwise until evolution of gas ceased. The resulting mixture was stirred for 1 h and then diluted with ethyl acetate (300 mL) and washed with brine. After drying (Na2SO4) the solvent was evaporated under reduced pressure to yield the crude title compound (16.7 g, 100%). (m/z)=439+441 (M+H)+.
Aufarbeitung
- stirringThe resulting mixture was stirred for 1 h
- washwashed with brine
- dry with materialAfter drying (Na2SO4) the solvent
- customwas evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-a157d25e50324c6e8598cc2405a31107
- Quelldatensatz
- uspto-grants-2011_08
- Patentnummer
- US07989442B2
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