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Water → 6-fluoro-2-(4-methoxybenzyl)-7-methylisoquinolin-1(2H)-one

HRID 1913132
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HRID 1913132 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[C:8](=[O:13])[NH:7][CH:6]=[CH:5]2.C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:20][O:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26]Cl)=[CH:24][CH:23]=1.O>CN(C=O)C.CCCCCCC.C(OCC)(=O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[C:8](=[O:13])[N:7]([CH2:26][C:25]1[CH:28]=[CH:29][C:22]([O:21][CH3:20])=[CH:23][CH:24]=1)[CH:6]=[CH:5]2
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참가 물질

7

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 699934-Methyloxybenzyl chlorideHCID 592260506-Fluoro-7-methylisoquinolin-1(2H)-one

생성물 1

HCID 592260436-fluoro-2-(4-methoxybenzyl)-7-methylisoquinolin-1(2H)-one

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 21899848Ethylacetate heptane용매

실험 절차

To a solution of 9.17 g (51.8 mmol) of 6-fluoro-7-methyl-2H-isoquinolin-1-one in 80 ml of DMF were added 20.2 g (62.1 mmol) of cesium carbonate and then 8.92 g (56.9 mmol) of 4-methoxybenzylchloride. After stirring at room temperature for 90 minutes the reaction mixture was poured into 600 ml of water, stirred for 1 h, and then the precipitated product was isolated by suction. From the mother liquor additional producted was isolated by chromatography with heptane/ethyl acetate (80:20). The combined products were recrystallized from ethyl acetate and 8.39 g 6-fluoro-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one were received.

후처리

  1. stirringstirred for 1 h
  2. customthe precipitated product was isolated by suction
  3. customThe combined products were recrystallized from ethyl acetate and 8.39 g 6-fluoro-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one

출처 및 근거

ORD 기록
ord-298a55d9ce41469fba8f0e0665a598cb
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08609691B2

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