3-(4-Aminophenyl)propionic acid → 4-Aminobenzenepropanol
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10](O)=[O:11])=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][OH:11])=[CH:6][CH:7]=1参加物
4
実験手順
To an oven-dried 150 mL round-bottomed flask charged with 3-(4-aminophenyl)propionic acid (Aldrich, 3.0 g, 18.16 mmol) was added THF (50 mL) and lithium aluminum hydride (Aldrich, 1.0M THF solution, 37 mL, 36.32 mmol) at 0° C. The reaction mixture was added Na2SO4.10H2O after 3 h until there was no visible bubbles. The liquid was filtered. The solid was washed with THF and CH2Cl2. The filtrate was dried over Na2SO4. After filtration and concentration in vacuo, the crude was purified by flash chomatography (7% MeOH—CH2Cl2) to provide the title product. MS (ESI): 152 (M+H)+.
後処理
- filtrationThe liquid was filtered
- washThe solid was washed with THF and CH2Cl2
- dry with materialThe filtrate was dried over Na2SO4
- filtrationAfter filtration and concentration in vacuo
- customthe crude was purified by flash chomatography (7% MeOH—CH2Cl2)
出典と根拠
- ORDレコード
- ord-0948143fff634beab2c395645f8ae67d
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07662811B2
反応ノート
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