HCID 45088409、化合物 → [(2S)-1-Methylpyrrolidin-2-yl]acetonitrile

HRID 497074ノート

反応式

HRID 497074 の反応式
[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

反応物 1

HCID 45088409HCID 45088409、化合物

生成物 1

HCID 12648940[(2S)-1-Methylpyrrolidin-2-yl]acetonitrile

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

Raney-Ni (1.5 ml) was added to an EtOH (30 ml) solution of the 2-((2S)-1-methyl-5-thioxopyrrolidin-2-yl)ethanenitrile (940 mg, 6.1 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-((2S)-1-methylpyrrolidin-2-yl)ethanenitrile as a mixture (195 mg) with impurities difficult to separate.

後処理

  1. temperaturethe mixture was heated for 24 hours
  2. temperatureunder reflux (upon TCL
  3. filtrationThe inorganic matter was filtered off
  4. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-5d80ff94621648ffb2825c37a91dc7d3
出典データセット
uspto-grants-2005_09
特許番号
US06949553B2

反応ノート

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