Sodium Chloride → HCID 67225376、化合物

HRID 2367880

反応式

HRID 2367880 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-].[NH4+:12].[C-:13]#[N:14].[Na+].[Cl-].[Na+]>N>[NH2:12][C:6]1([C:13]#[N:14])[CH2:7][CH2:8][N:3]([N:2]([CH3:10])[CH3:1])[CH2:4][CH2:5]1

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 567377821-(Dimethylamino)-4-piperidinone

生成物 1

HCID 67225376HCID 67225376、化合物

試薬・触媒・溶媒 1

HCID 222Ammonia溶媒

実験手順

6.3 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) is dissolved in 135 ml aqueous ammonia (25%). To this solution 3.55 g ammonium chloride is added, then 4.34 g sodium cyanide. The reaction mixture is stirred at room temperature for 18 hours. Then the mixture is saturated with sodium chloride, and four times extracted with ethyl acetate. The organic layer is dried over sodium sulfate, and the solvent is evaporated, to yield 5.6 g 4-Amino-1-dimethylamino-piperidine-4-carbonitrile as a yellow oil. 1H-NMR (CDCl3): 2.95 ppm (m, 2H), 2.65 ppm (m, 2H), 2.40 ppm (s, 6H), 2.05 ppm (m, 2H), 1.80 ppm (m, 2H), 1.75 ppm (s, broad, 2H).

後処理

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

出典と根拠

ORDレコード
ord-a2581c7f0c7e42fb9f16515d00b2bf06
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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