4-Pyridinepropaneamide → 4-Pyridinepropanenitrile

HRID 364717

反応式

HRID 364717 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][C:9]([NH2:11])=O)=[CH:3][CH:2]=1>O=P(Cl)(Cl)Cl>[C:9]([CH2:8][CH2:7][C:4]1[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=1)#[N:11]

参加物

3

反応物 1

HCID 37782334-Pyridinepropaneamide

生成物 1

HCID 73304614-Pyridinepropanenitrile収率 77%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture of 3-(4-pyridyl)-propionamide (7.1 g, 0.47M) in POCl3 (25 ml) was heated at about 100° to about 110° C. for 2 hrs. The excess of POCl3 was removed in vacuo from the reaction. Thereafter water was added and the resulting solution was basified with aqueous Na2CO3 sol. and extracted with CHCl3. The combined extracts were dried over Na2SO4 and concentrated and distilled at 1 mmHg/118°-120° C. to give 4(2-cyanoethyl)pyridine as an oil (4.8 g, 77% yield).

後処理

  1. temperaturewas heated at about 100° to about 110° C. for 2 hrs
  2. customThe excess of POCl3 was removed in vacuo from the reaction
  3. additionThereafter water was added
  4. extractionextracted with CHCl3
  5. dry with materialThe combined extracts were dried over Na2SO4
  6. concentrationconcentrated
  7. distillationdistilled at 1 mmHg/118°-120° C.

出典と根拠

ORDレコード
ord-f4fbddcfe74a42fbb1968b95d9344d80
出典データセット
uspto-grants-1986_08
特許番号
US04605744

関連ノート

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