反応式
[CH2:1]([O:8][C@H:9]([C:22]([F:25])([F:24])[F:23])[C@@H:10]([NH:14]C(OC(C)(C)C)=O)[C:11]([OH:13])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:26]>CCOC(C)=O>[ClH:26].[NH2:14][C@H:10]([C@H:9]([O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:22]([F:24])([F:25])[F:23])[C:11]([OH:13])=[O:12]参加物
4
実験手順
To a solution of (2R,3S)-3-(benzyloxy)-2-(tert-butoxycarbonylamino)-4,4,4-trifluorobutanoic acid (1.56 g, 4.2 mmol) in EtOAc (30 mL) was added EtOAc saturated with hydrogen chloride (30 mL) at 0° C. Then, the mixture was stirred at room temperature for 1.5 h. After concentration of the reaction mixture to about 15 mL, the white solid was collected by filtration and washed with EtOAc, dried in vacuum to give the title compound (2R,3S)-2-amino-3-(benzyloxy)-4,4,4-trifluorobutanoic acid hydrochloride salt (1.06 g, 84% for two steps). 1H NMR (400 MHz, CD3OD, δ in ppm) 7.32˜7.44 (m, 5H), 4.86 (d, J=2.0 Hz, 2H), 4.70 (dq, J=3.6, 6.6 Hz, 1H), 4.50 (d, J=3.6 Hz, 1H).
後処理
- filtrationAfter concentration of the reaction mixture to about 15 mL, the white solid was collected by filtration
- washwashed with EtOAc
- customdried in vacuum
出典と根拠
- ORDレコード
- ord-050d1ef4519a4eb4abb6c3f1a88031c6
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642632B2
関連ノート
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