HCID 45088408、化合物 → HCID 12648939、化合物
反応式
[CH3:1][N:2]1[C:6](=S)[CH2:5][CH2:4][C@@H:3]1[CH2:8][C:9]#[N:10]>[Ni].CCO>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][C@@H:3]1[CH2:8][C:9]#[N:10]参加物
4
実験手順
Raney-Ni (1.5 ml) was added to an EtOH (30 ml) solution of the 2-((2R)-1-methyl-5-thioxopyrrolidin-2-yl)ethanenitrile (1.36 g, 8.8 mmols), and the mixture was heated for 24 hours under reflux (Upon TCL, the starting materials had not completely disappeared). The inorganic matter was filtered off, and then the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (SiO2 40 g, MeOH—CHCl3 1:9 v/v) to obtain 2-((2R)-1-methylpyrrolidin-2-yl)ethanenitrile as a mixture (498 mg) with impurities difficult to separate.
後処理
- temperaturethe mixture was heated for 24 hours
- temperatureunder reflux (Upon TCL
- filtrationThe inorganic matter was filtered off
- distillationthe solvent was distilled off under reduced pressure
出典と根拠
- ORDレコード
- ord-0ac0d5d068e34cf2a7fa6d5e9dc9d04b
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06949553B2
反応ノート
読み込み中…