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Cesium fluoride → HCID 71742701, 화합물

HRID 1852115
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인쇄 미리보기

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HRID 1852115 반응식
Cl[C:2]1[C:11]2[C:6](=[C:7]([O:13][CH3:14])[CH:8]=[C:9]([F:12])[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[F-:15].[Cs+]>CS(C)=O.CCOC(C)=O>[F:15][C:2]1[C:11]2[C:6](=[C:7]([O:13][CH3:14])[CH:8]=[C:9]([F:12])[CH:10]=2)[CH:5]=[CH:4][N:3]=1
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참가 물질

5

반응물 2

HCID 25953Cesium fluorideHCID 717427031-Chloro-7-fluoro-5-methoxyisoquinoline

생성물 1

HCID 71742701HCID 71742701, 화합물수율 105.3%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

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온도
140 °C

실험 절차

To a solution of 1-chloro-7-fluoro-5-methoxyisoquinoline (350 mg, 1.654 mmol) in DMSO (3 mL), was added CsF (502 mg, 3.31 mmol) and the mixture was heated to 140° C. for 4 h. The reaction was diluted with EtOAc and washed with water, and brine. The organic phase was collected, dried over sodium sulfate, and concentrated under vacuum to give 1,7-difluoro-5-methoxyisoquinoline (340 mg, 105% yield) which was not purified further. MS m/z 196.1 (M++1).

후처리

  1. washwashed with water, and brine
  2. customThe organic phase was collected
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-c10dbc402c364ccd93f8463e129ce2f9
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08957203B2

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