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

HRID 1022369

反応式

HRID 1022369 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2 回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 (J. Org. Chem. 1961, 26, 1867-74) in 240 ml ammoniumhydroxide 25% in water there are added 6.2 g of ammoniumchloride and 4.6 g of sodium cyanide. After stirring for 18 h at 25° C. the reaction mixture is diluted with 200 ml water and extracted with ethyl acetate. The organic phase is separated, dried over sodium sulphate, filtered and evaporated. 8.25 g of 4-amino-1-methoxy-piperidine-4-carbonitrile is obtained as light brow oil, which is used without further purification in the next step.

後処理

  1. extractionextracted with ethyl acetate
  2. customThe organic phase is separated
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-f4e338df5ee04a02bd6e4dab3868329c
出典データセット
uspto-grants-2014_05
特許番号
US08722578B2

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