Hydrochloric Acid → cyclopropyl-(R)-1-pyrrolidin-2-ylmethyl-amine
反応式
[CH:1]1([NH:4][C:5]([C@H:7]2[CH2:11][CH2:10][CH2:9][NH:8]2)=O)[CH2:3][CH2:2]1.Cl>C1COCC1>[CH:1]1([NH:4][CH2:5][C@H:7]2[CH2:11][CH2:10][CH2:9][NH:8]2)[CH2:3][CH2:2]1参加物
4
実験手順
(R)-Pyrrolidine-2-carboxylic acid cyclopropylamide (0.5 g, 3.2 mmol) in THF (4 mL) was added to borane-tetrahydrofuran complex (6 mL, 1 M, 6 mmol) at 0° C. The reaction mixture was refluxed for overnight after which more BH3 was added and heating was continued for another 2 h. The reaction mixture was acidified with 3M HCl soution and refluxed for 0.5 h. The reaction mixture was concentrated and the residue was basified with 2M NaOH solution. It crude reaction mixture was then extracted with 5% methanol in dichloromethane to give 0.4 g (89%) of cyclopropyl-(R)-1-pyrrolidin-2-ylmethyl-amine.
後処理
- temperatureThe reaction mixture was refluxed for overnight after which more
- additionwas added
- temperatureheating
- temperaturerefluxed for 0.5 h
- concentrationThe reaction mixture was concentrated
- customIt crude reaction mixture
- extractionwas then extracted with 5% methanol in dichloromethane
出典と根拠
- ORDレコード
- ord-b1898f5138054662b97a8edf331b9543
- 出典データセット
- uspto-grants-2003_07
- 特許番号
- US06599902B2
反応ノート
読み込み中…