Potassium Carbonate → methyl 2-(5-bromo-2-oxopyridin-1(2H)-yl)acetate

HRID 919291

반응식

HRID 919291 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([OH:8])=[N:6][CH:7]=1.Br[CH2:10][C:11]([O:13][CH3:14])=[O:12].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[N:6]([CH2:10][C:11]([O:13][CH3:14])=[O:12])[CH:7]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 178515818HCID 178515818, 화합물

생성물 1

HCID 28834262methyl 2-(5-bromo-2-oxopyridin-1(2H)-yl)acetate

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
60 °C

실험 절차

A mixture of 5-bromopyridin-2-ol (100 mg, 0.57 mmol), methyl 2-bromoacetate (168 mg, 1.1 mmol) and potassium carbonate (238 mg, 1.7 mmol) in acetone (5 mL) was stirred at 60° C. for 3 h. The solution was allowed to cool to room temperature, filtered and the filter cake was washed with acetone (5 mL×2). The filtrate was collected and concentrated under reduced pressure to give the crude product, which was purified by silica gel column chromatography (PE: EA=15:1) to afford the title compound: LC/MS m/z=246.1 [M+H]+

후처리

  1. temperatureto cool to room temperature
  2. filtrationfiltered
  3. washthe filter cake was washed with acetone (5 mL×2)
  4. customThe filtrate was collected
  5. concentrationconcentrated under reduced pressure
  6. customto give the crude product, which
  7. customwas purified by silica gel column chromatography (PE: EA=15:1)

출처 및 근거

ORD 기록
ord-533fe365af6243879bca6a64e34b8f94
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273033B2

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