2-Bromoethanol → 2-[(5-Methylpyridin-2-yl)oxy]ethanol

HRID 1097259ノート

反応式

HRID 1097259 の反応式
Br[CH2:2][CH2:3][OH:4].[OH:5][C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][N:7]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[CH3:12][C:9]1[CH:10]=[CH:11][C:6]([O:5][CH2:2][CH2:3][OH:4])=[N:7][CH:8]=1

参加物

6

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 178426911HCID 178426911、化合物

生成物 1

HCID 207951692-[(5-Methylpyridin-2-yl)oxy]ethanol

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A suspension of 0.291 ml (4.12 mmol) of 2-bromoethanol, of 0.3 g (2.75 mmol) of 2-hydroxy-5-methylpyridine and of 0.85 g (6.18 mmol) of potassium carbonate in 3 ml of dimethylformamide is vigorously stirred for 12 hours at reflux. The mixture is subsequently diluted with 100 ml of water and extracted with 100 ml of dichloromethane. The organic phase is washed with 50 ml of water, dried over sodium sulphate, concentrated under reduced pressure and then chromatographed on a silica column, elution being carried out with a mixture of hexane and ethyl acetate. The expected product is thus isolated.

後処理

  1. temperatureat reflux
  2. extractionextracted with 100 ml of dichloromethane
  3. washThe organic phase is washed with 50 ml of water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated under reduced pressure
  6. customchromatographed on a silica column, elution
  7. additionbeing carried out with a mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-8965f48bb51349a691d45aacbc04b576
出典データセット
uspto-grants-2012_03
特許番号
US08143248B2

反応ノート

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