Sodium Cyanide → 4-Amino-1-methoxy-piperidine-4-carbonitrile

HRID 1962357ノート

反応式

HRID 1962357 の反応式
[CH3:1][O:2][N:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.[Cl-].[NH4+:11].[C-:12]#[N:13].[Na+]>[OH-].[NH4+].O>[NH2:11][C:6]1([C:12]#[N:13])[CH2:7][CH2:8][N:3]([O:2][CH3:1])[CH2:4][CH2:5]1

参加物

6

反応物 3

HCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 199366531-Methoxypiperidin-4-one

生成物 1

HCID 596145944-Amino-1-methoxy-piperidine-4-carbonitrile収率 68.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14923Ammonium Hydroxide溶媒

反応条件

温度
25 °C

実験手順

To 10 g of N-methoxy-4-piperidone (Journal of Organic Chemistry (1961), 26, 1867-74) in 240 ml of ammonium hydroxide (25% in water) was added 6.2 g of ammonium chloride and 4.6 g of sodium cyanide. After stirring for 18 hours at 25° C. the reaction mixture was diluted with 200 ml of water and extracted with ethyl acetate. The organic phase was separated, dried over sodium sulfate and evaporated. 8.25 g of 4-amino-1-methoxy-piperidine-4-carbonitrile was obtained as a light brown oil, which was used without further purification in the next step.

後処理

  1. extractionextracted with ethyl acetate
  2. customThe organic phase was separated
  3. dry with materialdried over sodium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-6f889f405fcb447ab51798719fd853e6
出典データセット
uspto-grants-2013_04
特許番号
US08415369B2

反応ノート

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