Reaktionsgleichung
[C:1]1(=[N:11]O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.[OH2:13]>>[NH:11]1[C:6](=[O:13])[CH2:7][CH2:8][CH2:9][C:10]2[CH:5]=[CH:4][CH:3]=[CH:2][C:1]1=2Komponenten
3
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
To 3,4-dihydro-2H-naphthalen-1-one oxime (5 g, 31 mmol), PPA (50 g) was added and the mixture was heated at 120° C. for 4.5 hrs. While hot the mixture was quenced in a slurry of ice and water and vigorously stirred until a precipitate formed. The precipitate was filtered and rinsed with water to yield 1,3,4,5-tetrahydrobenzo[b]azepin-2-one (3.1 g). MS [M+H]+: 162.0; tR=1.76 min. (method 1)
Aufarbeitung
- customformed
- filtrationThe precipitate was filtered
- washrinsed with water
Quellen und Nachweise
- ORD-Eintrag
- ord-4dd717a03e8f46acbe242e9b3cdaf2c8
- Quelldatensatz
- uspto-grants-2013_07
- Patentnummer
- US08481738B2
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