Phosphorus oxychloride → 1-Benzylpiperidine-4-carbonitrile

HRID 47330

반응식

HRID 47330 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([NH2:16])=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O>CN(C)C=O>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 7831561-Benzylpiperidine-4-carboxamide

생성물 1

HCID 7933831-Benzylpiperidine-4-carbonitrile수율 94.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5 ml N,N-dimethylformamide was added to a mixture of 12.7 g 1-benzyl-4-piperidine carboxamide and 60 ml phosphorus oxychloride under ice-cooling, and it was stirred at room temperature for 1.5 hr. It was evaporated, and the resulting residue was dissolved in ethyl acetate and washed with aqueous sodium hydroxide and brine. After drying over anhydrous sodium sulfate, it was evaporated, and the resulting residue was purified by silica gel column chromatography to give 11.0 g of 1-benzyl-4-piperidine carbonitrile.

후처리

  1. temperaturecooling
  2. customIt was evaporated
  3. dissolutionthe resulting residue was dissolved in ethyl acetate
  4. washwashed with aqueous sodium hydroxide and brine
  5. dry with materialAfter drying over anhydrous sodium sulfate, it
  6. customwas evaporated
  7. customthe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-96af40e9e890427598b15566fb3e39e9
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699870B2

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