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

HRID 1089435ノート

反応式

HRID 1089435 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59c3126467824be7ae7abe85ece5af9a
出典データセット
uspto-grants-1990_10
特許番号
US04966901

反応ノート

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