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

HRID 1022369

반응식

HRID 1022369 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 596145944-Amino-1-methoxy-piperidine-4-carbonitrile수율 68.7%

시약·촉매·용매 2

HCID 962Water용매2회HCID 14923Ammonium Hydroxide용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f4e338df5ee04a02bd6e4dab3868329c
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722578B2

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