Pyridine → HCID 12674764、化合物

HRID 67111ノート

反応式

HRID 67111 の反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].OCC[N:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1.N1C=CC=CC=1>O>[C:5]([O:4][CH2:1][CH2:2][N:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1)(=[O:7])[CH3:6]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic Anhydride2 回HCID 109754381-(2-Hydroxyethyl)pyrrole

生成物 1

HCID 12674764HCID 12674764、化合物収率 55%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The resulting product is reacted with acetic anhydride in accordance with the method of F. F. Blicheand E. S. Blake, J.Am.Chem.Soc.,53, 1015 (1931). A mixture of 1-(2-hydroxyethyl)pyrrole (147 g, 1.32 mole), pyridine (415 ml) and acetic anhydride (139 ml) is heated on a steam bath for 0.5 hours. The reaction mixture is cooled to room temperature, poured into water (one 1) and the product is extracted into ethyl acetate (3×1 l). The extract is washed successively with dilute hydrochloric acid, saturated sodium chloride solution, dilute sodium bicarbonate solution, and again with saturated sodium chloride solution. The extract is dried over sodium sulfate, evaporated in vacuo and the residue (150 g) is subjected to column chromatography on Florisil® activated magnesium silicate. The desired product is eluted with hexane-dichloromethane (1:1) to give 128 g (55%) 1-(2-acetoxyethyl)pyrrole, an oil, identical to an authentic specimen.

後処理

  1. temperatureis heated on a steam bath for 0.5 hours
  2. extractionthe product is extracted into ethyl acetate (3×1 l)
  3. washThe extract is washed successively with dilute hydrochloric acid, saturated sodium chloride solution, dilute sodium bicarbonate solution
  4. dry with materialThe extract is dried over sodium sulfate
  5. customevaporated in vacuo
  6. washThe desired product is eluted with hexane-dichloromethane (1:1)

出典と根拠

ORDレコード
ord-b60bc21ab9644a1b91ac904792649ac3
出典データセット
uspto-grants-1982_08
特許番号
US04344943

反応ノート

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