Phosphorus oxychloride → 1-Benzylpiperidine-4-carbonitrile

HRID 47330

反応式

HRID 47330 の反応式
[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

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 7831561-Benzylpiperidine-4-carboxamide

生成物 1

HCID 7933831-Benzylpiperidine-4-carbonitrile収率 94.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-96af40e9e890427598b15566fb3e39e9
出典データセット
uspto-grants-2004_03
特許番号
US06699870B2

関連ノート

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