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

HRID 2063284노트

반응식

HRID 2063284 반응식
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

참가 물질

6

반응물 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 178426911HCID 178426911, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8322950acbd24653be8bdf27323ff526
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288376B2

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