Hydrogen chloride-ethyl acetate → N-[(1S)-2-({1-[6-(2-cyclopropylethoxy)-1,3-benzoxazol-2-yl]piperidin-4-yl}oxy)-1-methylethyl]acetamide
反応式
[CH:1]1([CH2:4][CH2:5][O:6][C:7]2[CH:33]=[CH:32][C:10]3[N:11]=[C:12]([N:14]4[CH2:19][CH2:18][CH:17]([O:20][CH2:21][C@@H:22]([NH:24][C:25](=O)[O:26]C(C)(C)C)[CH3:23])[CH2:16][CH2:15]4)[O:13][C:9]=3[CH:8]=2)[CH2:3][CH2:2]1.Cl.[C:35](OCC)(=O)C>>[CH:1]1([CH2:4][CH2:5][O:6][C:7]2[CH:33]=[CH:32][C:10]3[N:11]=[C:12]([N:14]4[CH2:19][CH2:18][CH:17]([O:20][CH2:21][C@@H:22]([NH:24][C:25](=[O:26])[CH3:35])[CH3:23])[CH2:16][CH2:15]4)[O:13][C:9]=3[CH:8]=2)[CH2:2][CH2:3]1参加物
3
実験手順
To tert-butyl [(1S)-2-({1-[6-(2-cyclopropylethoxy)-1,3-benzoxazol-2-yl]piperidin-4-yl}oxy)-1-methylethyl]carbamate (5.84 g) was added 4M hydrogen chloride/ethyl acetate (50 mL), and the mixture was stirred at room temperature for 15 min, and concentrated. Pyridine (50 mL) and acetic anhydride (50 mL) were added to the residue, and the mixture was stirred at room temperature for 20 min. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (NH, ethyl acetate/hexane) and recrystallized from ethyl acetate/hexane to give the title compound (3.83 g) as white crystals.
後処理
- concentrationconcentrated
- additionPyridine (50 mL) and acetic anhydride (50 mL) were added to the residue
- stirringthe mixture was stirred at room temperature for 20 min
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue was purified by silica gel chromatography (NH, ethyl acetate/hexane)
- customrecrystallized from ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-48d5c38400aa46f3bdfe275462484bd3
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08703758B2
反応ノート
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