Pyridine → HCID 12674764, 화합물

HRID 638307노트

반응식

HRID 638307 반응식
[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]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7918Acetic Anhydride2회HCID 109754381-(2-Hydroxyethyl)pyrrole

생성물 1

HCID 12674764HCID 12674764, 화합물수율 55%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The resulting product is reacted with acetic anhydride in accordance with the method of F. F. Blicke and 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 l) 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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d10057da72b54615931db0b4cba4f144
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04560699

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