Potassium Cyanide → 1-Benzyl-4-(cyanomethyl)piperidine-4-carbonitrile

HRID 491470노트

반응식

HRID 491470 반응식
C(OC(=O)[C:5](=[C:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)[C:6]#[N:7])C.[C-:22]#[N:23].[K+]>CCO.O>[CH2:14]([N:11]1[CH2:10][CH2:9][C:8]([CH2:5][C:6]#[N:7])([C:22]#[N:23])[CH2:13][CH2:12]1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

참가 물질

5

반응물 2

HCID 9032Potassium CyanideHCID 424752Ethyl 2-(1-benzylpiperidin-4-ylidene)-2-cyanoacetate

생성물 1

HCID 128476541-Benzyl-4-(cyanomethyl)piperidine-4-carbonitrile수율 81.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of (1-benzyl-piperidin-4-ylidene)-cyano-acetic acid ethyl ester (112.9 g, 0.40 mol) in EtOH (500 ml) and H2O (100 ml), potassium cyanide (64.6 g, 0.99 mol) is added at ambient temperature. The reaction mixture is stirred at 65 C.° for 24 h. After removal of EtOH, H2O is added to the residue. The waster phase is extracted with diethyl ether. The combined extracts are washed with H2O and brine, dried over sodium sulfate and evaporated down to give 77.7 g of 1-benzyl-4-cyanomethyl-piperidine-4-carbonitrile.

후처리

  1. customAfter removal of EtOH, H2O
  2. additionis added to the residue
  3. extractionThe waster phase is extracted with diethyl ether
  4. washThe combined extracts are washed with H2O and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated down

출처 및 근거

ORD 기록
ord-d14765825f544761824cd3df324f0815
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531546B2

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