反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]([CH3:14])(O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(=O)(=O)(O)O.C(=O)([O-])[O-:21].[K+].[K+].ClCCl.[C:29](#[N:31])[CH3:30]>>[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]([NH:31][C:29](=[O:21])[CH3:30])([CH3:14])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
6
実験手順
To a solution of 1-benzyl-3-methylpyrrolidin-3-ol (1.0 g, 5.2 mmol) in acetonitrile (10 mL) at 0° C., was added concentrated sulfuric acid (10 mL) slowly. After being stirred for 16 hours at room temperature, the reaction mixture was poured into ice-water. After the reaction mixture was adjusted to pH 7 with a saturated aqueous solution of potassium carbonate, the resulting mixture was exacted with dichloromethane (200 mL×3). The combined organic layers were dried over sodium sulfate, and concentrated in vauo. The residue was purified by preparative HPLC to afford 600 mg of the product (yield was 50%).
後処理
- dry with materialThe combined organic layers were dried over sodium sulfate
- concentrationconcentrated in vauo
- customThe residue was purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-8ccc0ee2e02f400c8e620e39af55cf5b
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871756B2
関連ノート
読み込み中…