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

HRID 491461ノート

反応式

HRID 491461 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 128476541-Benzyl-4-(cyanomethyl)piperidine-4-carbonitrile収率 81.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dab84b2fcf074c6bb6a68688472e8a72
出典データセット
uspto-grants-2009_05
特許番号
US07531546B2

反応ノート

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