Water → (4-(Methoxymethyl)cyclohexyl)methanamine
反応式
[CH3:1][O:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH:7]([C:10]#[N:11])[CH2:6][CH2:5]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].O>O1CCCC1>[CH3:1][O:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][NH2:11])[CH2:6][CH2:5]1参加物
6
実験手順
To a solution of EXAMPLE 374D (460 mg) in tetrahydrofuran (15 mL) was added 2M lithium aluminum hydride in tetrahydrofuran (2.252 mL) slowly. The reaction mixture was stirred at room temperature for 1 hour, refluxed for 1 hour and cooled. 2 ml of 2M aqueous NaOH and water (5 mL) was added. The solid was filtered off and washed with ether. The filtrate was concentrated. The residue was mixed with dichloromethane (50 mL) and the resulting mixture was dried over Na2SO4 and concentrated to provide the title compound.
後処理
- temperaturerefluxed for 1 hour
- temperaturecooled
- filtrationThe solid was filtered off
- washwashed with ether
- concentrationThe filtrate was concentrated
- additionThe residue was mixed with dichloromethane (50 mL)
- dry with materialthe resulting mixture was dried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-ce1d17942c564c4fb6d2d1b785198c7a
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034875B2
反応ノート
読み込み中…