Methyl 2-(2-cyanophenoxy)acetate → 4,5-dihydro-1,4-benzoxazepin-3(2H)-one
反応式
[C:1]([C:3]1[CH:14]=[CH:13][CH:12]=[CH:11][C:4]=1[O:5][CH2:6][C:7](OC)=[O:8])#[N:2]>CO.[Ni]>[O:5]1[C:4]2[CH:11]=[CH:12][CH:13]=[CH:14][C:3]=2[CH2:1][NH:2][C:7](=[O:8])[CH2:6]1参加物
4
実験手順
The methanol solution of methyl (2-cyanophenoxy)acetate (40 g, 0.209 mol) was added to the mixture of Raney Ni (80 g) in 500 mL of methanol. The reaction mixture was stirred at room temperature overnight under hydrogen atmosphere. Raney Ni was removed by filtration, and the filtrated was concentrated under reduced pressure to give a residue which was purified by column chromatography on silica gel (methanol/dichloromethane, 1:50) to give 23 g of product. MS obsd. (ESI+) [(M+H)+] 164.
後処理
- customRaney Ni was removed by filtration
- concentrationthe filtrated was concentrated under reduced pressure
- customto give a residue which
- customwas purified by column chromatography on silica gel (methanol/dichloromethane, 1:50)
出典と根拠
- ORDレコード
- ord-50ee3a4e7691456db08c075c646dc4e7
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871756B2
反応ノート
読み込み中…