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Imidazole → HCID 22409067、化合物

HRID 1176426
ノート
印刷プレビュー

反応式

HRID 1176426 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[H-].[Na+].Cl[CH2:9][CH2:10][CH2:11][O:12][CH3:13]>CN(C)C=O>[CH3:13][O:12][CH2:11][CH2:10][CH2:9][N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 795ImidazoleHCID 24758Sodium hydrideHCID 1189271-Chloro-3-methoxypropane

生成物 1

HCID 22409067HCID 22409067、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

The mixture of 5.02 g of imidazole and 50 ml of N,N-dimethylformamide is admixed at 0° C. with 3.52 g of sodium hydride dispersion (69%) and stirred at room temperature over 1 hour. The solution of 8.36 g of 1-chloro-3-methoxypropane in 10 ml of N,N-dimethylformamide is added and the reaction solution is subsequently stirred at 60° C. over 2 hours. The reaction mixture is cooled, poured onto ice-water (150 ml) and extracted with ethyl acetate (3×150 ml). The organic phases are washed with water (3×150 ml) and brine (150 ml), dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained as a colourless oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.25 (200:20:1 dichloromethane-methanol-conc. ammonia); Rt=1.55.

後処理

  1. stirringthe reaction solution is subsequently stirred at 60° C. over 2 hours
  2. temperatureThe reaction mixture is cooled
  3. additionpoured onto ice-water (150 ml)
  4. extractionextracted with ethyl acetate (3×150 ml)
  5. washThe organic phases are washed with water (3×150 ml) and brine (150 ml)
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-146701fa8c794ecd9df3b7f141924cdc
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842688B2

反応ノート

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