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Potassium Carbonate → 6-Bromo-2H-pyrido[3,2-B][1,4]oxazin-3(4H)-one

HRID 1054913
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HRID 1054913 반응식
C[O:2][C:3](=O)[CH2:4][O:5][C:6]1[C:7]([NH2:13])=[N:8][C:9]([Br:12])=[CH:10][CH:11]=1.C([O-])([O-])=O.[K+].[K+]>CO>[Br:12][C:9]1[CH:10]=[CH:11][C:6]2[O:5][CH2:4][C:3](=[O:2])[NH:13][C:7]=2[N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 90011309HCID 90011309, 화합물

생성물 1

HCID 218737726-Bromo-2H-pyrido[3,2-B][1,4]oxazin-3(4H)-one

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

(2-Amino-6-bromopyridin-3-yloxy)acetic acid methyl ester (4.0 g, 15 mmol) was dissolved in MeOH (40 mL). K2CO3 (3.0 g, 22 mmol) was added and the reaction was stirred at 70° C. for 1 hour. Then, the solvent was removed under reduced pressure and the resulting slurry was suspended in dichloromethane (DCM) and washed with H2O and then brine. The organic layer was dried (Na2SO4) and the product was precipitated from DCM/Et2O to give 6-bromo-4H-pyrido[3,2-b][1,4]oxazin-3-one. Yield 1.9 g (8.3 mmol, 55%). LCMS (ESI): calc. C7H5BrN2O2=228, 230; obs. M+H=229, 231.

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. customThen, the solvent was removed under reduced pressure
  2. washwashed with H2O
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customthe product was precipitated from DCM/Et2O

출처 및 근거

ORD 기록
ord-bea06c556a2b437e94b068a91e2a0763
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394315B2

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