Triethylamine → Oxime-2,3-dihydro-6-methoxy-1H-inden-1-one
反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][C:9]2=O)=[CH:5][CH:4]=1.CCN(CC)CC.[NH2:20][OH:21].Cl>CO>[OH:21]/[N:20]=[C:9]1\[CH2:8][CH2:7][C:6]2[C:10]\1=[CH:11][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2参加物
5
実験手順
To a stirred suspension of 6-methoxy-2,3-dihydro-1H-inden-1-one (15.0 g, 93.0 mmol) and Et3N (28.2 g, 279 mmol) in MeOH (200 mL) was added NH2OH.HCl (12.8 g, 186 mmol) at room temperature. After the addition, the resulting solution was stirred at room temperature for 24 hours. The reaction mixture was concentrated under vacuum. To the residue was added EtOAc (300 mL). The solution was washed with water (2×150 mL), brine (150 mL), dried over Na2SO4, and concentrated under vacuum to give (1E)-N-hydroxy-6-methoxy-2,3-dihydro-1H-inden-1-imine (1a, 17 g, >100%) as a white solid.
後処理
- additionAfter the addition
- concentrationThe reaction mixture was concentrated under vacuum
- additionTo the residue was added EtOAc (300 mL)
- washThe solution was washed with water (2×150 mL), brine (150 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-221cb89194ec415ebf97b95dabe3f827
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040515B2
反応ノート
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