Hydrochloric Acid → (E)-(S)-5-Amino-2-(3-fluoropropyl)hex-2-enedioic acid
反応式
C(OC([NH:8][C@H:9]([C:22]([O:24]C(C)(C)C)=[O:23])[CH2:10]/[CH:11]=[C:12](\[CH2:18][CH2:19][CH2:20][F:21])/[C:13]([O:15]CC)=[O:14])=O)(C)(C)C.Cl>O>[NH2:8][C@H:9]([C:22]([OH:24])=[O:23])[CH2:10]/[CH:11]=[C:12](\[CH2:18][CH2:19][CH2:20][F:21])/[C:13]([OH:15])=[O:14]参加物
4
実験手順
A mixture of 6-tert-Butyl 1-ethyl (E)-(S)-5-[(tert-butoxycarbonyl)amino]-2-(3-fluoropropyl)hex-2-enedioate (1e) (80.0 mg, 0.20 mmol) and 4 N aqueous hydrochloric acid (1 mL) was heated to reflux for 4 h. The mixture was then cooled to r.t., diluted with water (5 mL) and lyophilised. The crude product was purified by preparative HPLC (XBridge C18, 5 μm 150×19 mm, acetonitrile/water (0.1% TFA) gradient, 21 mL/min). Yield: 12.0 mg, 0.04 mmol, 19%.
後処理
- temperaturewas heated
- temperatureto reflux for 4 h
- customThe crude product was purified by preparative HPLC (XBridge C18, 5 μm 150×19 mm, acetonitrile/water (0.1% TFA) gradient, 21 mL/min)
出典と根拠
- ORDレコード
- ord-d786353c42d54b028e90030b8695df1b
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09017645B2
反応ノート
読み込み中…