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Potassium Carbonate → 4-(4-Bromo-2-fluoro-phenoxy)-2,6-dimethyl-pyridine

HRID 889640
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인쇄 미리보기

반응식

HRID 889640 반응식
Br[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH3:9])[CH:3]=1.[Br:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[C:13]([F:18])[CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CCOC(C)=O>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][C:2]2[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH3:9])[CH:3]=2)=[C:13]([F:18])[CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27249814-Bromo-2-fluorophenolHCID 130817354-Bromo-2,6-dimethylpyridine

생성물 1

HCID 592873134-(4-Bromo-2-fluoro-phenoxy)-2,6-dimethyl-pyridine

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
150 °C

실험 절차

A mixture of 4-bromo-2,6-dimethyl-pyridine (1 g, 5.4 mmol), 4-bromo-2-fluoro-phenol (0.59 g, 5.4 mmol) and potassium carbonate (0.89 g, 6.4 mmol) in xylenes (2 ml) was heated at 150° C. (oil bath temperature) into a sealed tube for 48 hours. After cooling to room temperature the mixture was diluted with EtOAc and filtered through a diatomaceous earth pad. The filtrate was evaporated till dryness and the crude product thus obtained was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 10% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate D22 (1.28 g, 80%).

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. filtrationfiltered through a diatomaceous earth pad
  3. customThe filtrate was evaporated till dryness

출처 및 근거

ORD 기록
ord-e2ef77438c8d4e2f953cc50538716b3e
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252937B2

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