Hydrogen chloride-ethyl acetate → N-[(1S)-2-({1-[5-(cyclobutylmethoxy)-1,3-benzoxazol-2-yl]piperidin-4-yl}oxy)-1-methylethyl]acetamide
反応式
[CH:1]1([CH2:5][O:6][C:7]2[CH:8]=[CH:9][C:10]3[O:14][C:13]([N:15]4[CH2:20][CH2:19][CH:18]([O:21][CH2:22][C@@H:23]([NH:25][C:26](=[O:32])OC(C)(C)C)[CH3:24])[CH2:17][CH2:16]4)=[N:12][C:11]=3[CH:33]=2)[CH2:4][CH2:3][CH2:2]1.Cl.[C:35](OCC)(=O)C>>[CH:1]1([CH2:5][O:6][C:7]2[CH:8]=[CH:9][C:10]3[O:14][C:13]([N:15]4[CH2:16][CH2:17][CH:18]([O:21][CH2:22][C@@H:23]([NH:25][C:26](=[O:32])[CH3:35])[CH3:24])[CH2:19][CH2:20]4)=[N:12][C:11]=3[CH:33]=2)[CH2:2][CH2:3][CH2:4]1参加物
3
実験手順
To tert-butyl [(1S)-2-({1-[5-(cyclobutylmethoxy)-1,3-benzoxazol-2-yl]piperidin-4-yl}oxy)-1-methylethyl]carbamate (380 mg) was added 4M hydrogen chloride/ethyl acetate (5 mL), and the mixture was stirred at room temperature for 15 min and concentrated. Pyridine (5 mL) and acetic anhydride (5 mL) were added to the residue, and the mixture was stirred at room temperature for 10 min. After concentration, the residue was purified by silica gel chromatography (NH, hexane/ethyl acetate), and the obtained solid was washed with diethyl ether to give the title compound (158 mg).
後処理
- concentrationconcentrated
- additionPyridine (5 mL) and acetic anhydride (5 mL) were added to the residue
- stirringthe mixture was stirred at room temperature for 10 min
- concentrationAfter concentration
- customthe residue was purified by silica gel chromatography (NH, hexane/ethyl acetate)
- washthe obtained solid was washed with diethyl ether
出典と根拠
- ORDレコード
- ord-041e242e995344288e2e3ce6cafba9cc
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08703758B2
反応ノート
読み込み中…