Acetic Anhydride → 3-Acetyl-1-(2-acetylaminoethyl)-2,5-dimethylpyrrole

HRID 1089435노트

반응식

HRID 1089435 반응식
[C:1]([NH:4][CH2:5][CH2:6][N:7]1[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]1[CH3:13])(=[O:3])[CH3:2].[C:14](OC(=O)C)(=[O:16])[CH3:15].COCCOC>CCOCC.[Cl-].[Zn+2].[Cl-]>[C:14]([C:10]1[CH:9]=[C:8]([CH3:13])[N:7]([CH2:6][CH2:5][NH:4][C:1](=[O:3])[CH3:2])[C:11]=1[CH3:12])(=[O:16])[CH3:15]

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 80711,2-DimethoxyethaneHCID 13770049N-(2-(2,5-Dimethyl-1H-pyrrol-1-yl)ethyl)acetamide

생성물 1

HCID 145367523-Acetyl-1-(2-acetylaminoethyl)-2,5-dimethylpyrrole

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 3283Diethyl Ether용매2회

실험 절차

13.7 g (0.1 mol) of anhydrous zinc chloride are dissolved in 100 ml of ether and the solution is added to 18.0 g (0.1 mol) of 1-(2-acetylaminoethyl)-2,5-dimethylpyrrole and 9.5 ml (0.1 mol) of acetic anhydride in 50 ml of ether. After 1 hour at room temperature, 50 ml of ethylene glycol dimethyl ether are added and stirring is continued for 20 hours. After the hydrolysis, the organic phase is concentrated, the residue is chromatographed and the product is recrystallized from ethyl acetate.

후처리

  1. waitis continued for 20 hours
  2. customAfter the hydrolysis
  3. concentrationthe organic phase is concentrated
  4. customthe residue is chromatographed
  5. customthe product is recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-59c3126467824be7ae7abe85ece5af9a
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04966901

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