Sodium Hydroxide → 3-Methylindan-1-one oxime
反応式
[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=O)[CH2:3]1.Cl.[NH2:13][OH:14].[OH-].[Na+]>CO.O>[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[N:13][OH:14])[CH2:3]1参加物
6
反応条件
- 温度
- 80 °C
実験手順
To a solution of 3-methylindan-1-one (221 mg, 1.51 mmol) and hydroxylamine hydrochloride (295 mg, 4.25 mmol) in MeOH (4.00 mL) was added a solution of NaOH (200 mg, 5.00 mmol) in H2O (2.00 mL) and the mixture was stirred at 80° C. for 2 h. The cooled reaction was concentrated in vacuo to remove most of the MeOH, and the residue was partitioned between DCM and H2O. The organic layer was concentrated in vacuo to afford the title compound as a waxy solid (232 mg, 95%). LC/MS: Rt=1.51 min, ES+ 162 (AA standard).
後処理
- customThe cooled reaction
- concentrationwas concentrated in vacuo
- customto remove most of the MeOH
- customthe residue was partitioned between DCM and H2O
- concentrationThe organic layer was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-4b3ece9ae9484bfd8bffe453d0cc7e8c
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481550B2
反応ノート
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