Water → 2,2-Dimethyl-3-(4-pyridin-3-yl-imidazol-1-yl)-propyl acetate

HRID 432571ノート

反応式

HRID 432571 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:8]=[CH:9][NH:10][CH:11]=2)[CH:2]=1.[OH-].[K+].[C:14]([O:17][CH2:18][C:19]([CH3:23])([CH3:22])[CH2:20]Br)(=[O:16])[CH3:15].O>CS(C)=O.C(Cl)(Cl)Cl>[C:14]([O:17][CH2:18][C:19]([CH3:23])([CH3:22])[CH2:20][N:10]1[CH:11]=[C:7]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[N:8]=[CH:9]1)(=[O:16])[CH3:15]

参加物

7

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 133577153-Bromo-2,2-dimethylpropyl acetateHCID 178420772HCID 178420772、化合物

生成物 1

HCID 545188152,2-Dimethyl-3-(4-pyridin-3-yl-imidazol-1-yl)-propyl acetate

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6212Chloroform溶媒

反応条件

温度
70 °C

実験手順

To a solution of 4-pyridin-3-yl-imidazole (50 mg) in DMSO (1.7 mL) was added powered KOH (57 mg) and 3-bromo-2,2-dimethylpropyl acetate and the resulting suspension was heated at 70° C. for 48 hours. Water was added followed by CHCl3, the aqueous layer was extracted with CHCl3, the combined organic layers were washed with brine, dired over Na2SO4 and evaporated in vacuo. The residue was purified by preparative TLC (10% MeOH-90% CH2Cl2) the title compound as slightly yellow oil.

後処理

  1. extractionthe aqueous layer was extracted with CHCl3
  2. washthe combined organic layers were washed with brine
  3. customevaporated in vacuo
  4. customThe residue was purified by preparative TLC (10% MeOH-90% CH2Cl2) the title compound as slightly yellow oil

出典と根拠

ORDレコード
ord-acb142e284154a0bbf859dcb7908e8a6
出典データセット
uspto-grants-2003_12
特許番号
US06664238B1

反応ノート

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