Potassium Cyanide → HCID 86671305、化合物

HRID 2367890

反応式

HRID 2367890 の反応式
[CH3:1][N:2]([CH3:11])[N:3]1[CH2:8][CH2:7][C:6](=[N:9][OH:10])[CH2:5][CH2:4]1.P([O-])(O)(O)=O.[K+].[C-:18]#[N:19].[K+]>O>[CH3:1][N:2]([CH3:11])[N:3]1[CH2:8][CH2:7][C:6]([NH:9][OH:10])([C:18]#[N:19])[CH2:5][CH2:4]1

参加物

5

反応物 3

HCID 9032Potassium CyanideHCID 516951Monobasic potassium phosphateHCID 866713041-Dimethylamino-piperidin-4-one oxime

生成物 1

HCID 86671305HCID 86671305、化合物収率 53.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
5 °C

実験手順

12.4 g 1-Dimethylamino-piperidin-4-one oxime (from Step 1) is dissolved in 160 ml water. 49.3 g potassium dihydrogenphosphate is added. The resulting yellow suspension is cooled to 5° C., and a solution of 11.24 g potassium cyanide in 40 ml water is added. The mixture is stirred at room temperature for 2 days, then extracted with ethyl acetate, the organic layer dried over sodium sulfate, and the solvent evaporated, to give 7.8 g 1-Dimethylamino-4-hydroxyamino-piperidine-4-carbonitrile. 1H-NMR (CDCl3): 5.60 ppm (s, broad, 1H), 5.10 ppm (s, broad, 1H), 2.92 ppm (m, 2H), 2.61 ppm (m, 2H), 2.33 ppm (s, 6H), 2.10 ppm (m, 2H), 1.70 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-16d1c233e8934ee3b70bd591f0308c4d
出典データセット
uspto-grants-2014_04
特許番号
US08703165B2

関連ノート

読み込み中…