Methylamine → HCID 67225397、化合物

HRID 2367884

反応式

HRID 2367884 の反応式
[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.Cl.[CH3:12][NH2:13].[CH3:14][NH2:15].[C-]#N.[K+]>O>[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6]([NH:15][CH3:14])([C:12]#[N:13])[CH2:5][CH2:4]1

参加物

6

反応物 4

HCID 6329MethylamineHCID 9032Potassium CyanideHCID 6364545Methylamine hydrochlorideHCID 567377821-(Dimethylamino)-4-piperidinone

生成物 1

HCID 67225397HCID 67225397、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

5.5 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961), 4.2 g methylamine hydrochloride and 4.9 ml methylamine solution (40% in water) are mixed in 35 ml water, then to this mixture a solution of 4 g potassium cyanide in 10 ml water is added. The resulting mixture is stirred at room temperature for 3 days, then extracted with ethyl acetate, the organic layer dried over sodium sulfate, and the solvent evaporated. 5.3 g 1-Dimethylamino-4-methylamino-piperidine-4-carbonitrile is obtained. 1H-NMR (CDCl3): 2.86 ppm (m, 2H), 2.57 ppm (m, 2H), 2.44 ppm (s, 3H), 2.32 ppm (s, 6H), 2.00 ppm (m, 2H), 1.69 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-9cdbaf4bb1e74539b2d084de1c4c3ae6
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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