Hydrochloric Acid → (S)-t-Butyl 2-((hydroxyimino)methyl)pyrrolidine-1-carboxylate
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH2:10][C@H:9]1[CH:13]=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:16][OH:17].Cl>N1C=CC=CC=1>[OH:17][N:16]=[CH:13][C@@H:9]1[CH2:10][CH2:11][CH2:12][N:8]1[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7]参加物
5
実験手順
To a solution of (S)-t-butyl-2-formylpyrrolidine-1-carboxylate (40.94 g) in pyridine (411 mL), hydroxylamine monohydrochloride (28.56 g) was added at 0° C. and the mixture was stirred at room temperature for 17 hours. The reaction mixture was added to a mixture of AcOE (1.5 L) and hydrochloric acid (2 L, 3.0 N). The organic layer was separated, washed with saturated aqueous sodium bicarbonate (1 L), dried (MgSO4), filtered and concentrated to give the titled compound (39.78 g, colorless solid.)
後処理
- customThe organic layer was separated
- washwashed with saturated aqueous sodium bicarbonate (1 L)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-5c0f90933b1e4bd984f338bc22ecc4e6
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181229B2
反応ノート
読み込み中…