Potassium Cyanide → HCID 86671308、化合物

HRID 2367894

反応式

HRID 2367894 の反応式
[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.[C-:11]#[N:12].[K+].C(=O)([O-])O.[Na+]>ClCCl.O>[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6]([OH:9])([C:11]#[N:12])[CH2:5][CH2:4]1

参加物

6

反応物 3

HCID 9032Potassium CyanideHCID 516892Sodium BicarbonateHCID 567377821-(Dimethylamino)-4-piperidinone

生成物 1

HCID 86671308HCID 86671308、化合物収率 67.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 6.0 g 1-dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) in 30 ml of dichloromethane is added to a mixture of 4.1 g potassium cyanide and 10.6 g sodium hydrogencarbonate in 30 ml of water. The resulting mixture is stirred at room temperature for 3 hours, then extracted with ethyl acetate, the organic layer dried over sodium sulfate, and the solvent evaporated. 4.8 g 1-Dimethylamino-4-hydroxy-piperidine-4-carbonitrile is obtained. 1H-NMR (CDCl3): 3.95 ppm (s, broad, 1H), 2.90 ppm (m, 2H), 2.68 ppm (m, 2H), 2.40 ppm (s, 6H), 2.15 ppm (m, 2H), 1.95 ppm (m, 2H).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialthe organic layer dried over sodium sulfate
  3. customthe solvent evaporated

出典と根拠

ORDレコード
ord-61b3fabf40134bebaef07e460b75712f
出典データセット
uspto-grants-2014_04
特許番号
US08703165B2

関連ノート

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