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

HRID 58048
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인쇄 미리보기

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HRID 58048 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[NH:6][CH:7]=1.Br[CH2:10][C:11]([O:13][CH3:14])=[O:12].C([O-])([O-])=O.[K+].[K+]>CS(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
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 5995285-Bromo-2-hydroxypyridine

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
60 °C

실험 절차

To solution of 5-bromopyridin-2(1H)-one (2.5 g, 14.37 mmol) and methyl 2-bromoacetate (2.418 g, 15.81 mmol) in DMSO (12 mL) was added K2CO3 (2.383 g, 17.24 mmol). The mixture was stirred at 60° C. for 4 hours, filtered, and purified via preparative HPLC, eluting with a gradient of 10-90% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA) to give the title compound.

후처리

  1. filtrationfiltered
  2. custompurified via preparative HPLC
  3. washeluting with a gradient of 10-90% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA)

출처 및 근거

ORD 기록
ord-8a9a13226ab74f98ba60f664d65d6a8f
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434743B2

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