Acetic Acid → 2,3,4,5-Tetrahydro-1,4-benzoxazepin-9-ol hydrobromide
反応式
C[O:2][C:3]1[C:13]2[O:12][CH2:11][CH2:10][NH:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.C(O)(=O)C.C(OCC)C.[BrH:23]>>[BrH:23].[O:12]1[C:13]2[C:3]([OH:2])=[CH:4][CH:5]=[CH:6][C:7]=2[CH2:8][NH:9][CH2:10][CH2:11]1参加物
5
反応条件
- 温度
- 80 °C
実験手順
A suspension of 9-(methyloxy)-2,3,4,5-tetrahydro-1,4-benzoxazepine (Preparation 84) (43.4 g, 242 mmol) in 33% HBr in acetic acid (300 ml, 1823 mmol) was heated at 80° C. overnight. The mixture was allowed to cool to room temperature then treated with diethyl ether (300 ml) and stirred for 30 minutes. The resulting solid was collected by filtration, washed with diethyl ether (300 ml) and dried under vacuum at 40° C. to give the title compound as a pale brown powder (55.1 g)
後処理
- temperatureto cool to room temperature
- filtrationThe resulting solid was collected by filtration
- washwashed with diethyl ether (300 ml)
- customdried under vacuum at 40° C.
出典と根拠
- ORDレコード
- ord-476d3dbf87374b3c9e4bcdf5ebc98bdb
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08222245B2
反応ノート
読み込み中…