Hydrochloric Acid → (S)-2-(Pyrrolidin-2-yl)acetonitrile hydrochloride
反応式
[C:1]([CH2:3][C@@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1C(OC(C)(C)C)=O)#[N:2].[ClH:16]>CO>[ClH:16].[NH:5]1[CH2:6][CH2:7][CH2:8][C@H:4]1[CH2:3][C:1]#[N:2]参加物
4
反応条件
- 温度
- 40 °C
実験手順
A solution of tert-butyl (S)-2-cyanomethylpyrrolidine-1-carboxylate (Intermediate 139, 13.0 g) in methanol (130 mL) and concentrated hydrochloric acid (13 mL) was stirred and heated at 40° C. overnight. After cooling, the mixture was concentrated under vacuum and the residue was diluted with toluene and reconcentrated. Ethanol (20 mL) was added and the resultant solid was collected by filtration and washed with hexane to give ((S)-pyrrolidin-2-yl)acetonitrile hydrochloride (8.0 g) as a white solid.
後処理
- temperatureAfter cooling
- concentrationthe mixture was concentrated under vacuum
- additionthe residue was diluted with toluene
- additionEthanol (20 mL) was added
- filtrationthe resultant solid was collected by filtration
- washwashed with hexane
出典と根拠
- ORDレコード
- ord-b7812456ee8848e285e578d2e1c658e1
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09290472B2
反応ノート
読み込み中…