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Methyl iodide → 7-Benzyloxy-3-(4-chlorophenyl)-2-isopropyl-8-methoxy-chromen-4-one

HRID 14465
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HRID 14465 반응식
[CH2:1]([O:8][C:9]1[C:18]([OH:19])=[C:17]2[C:12]([C:13](=[O:30])[C:14]([C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=3)=[C:15]([CH:20]([CH3:22])[CH3:21])[O:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.IC.[C:33]([O-])([O-])=O.[K+].[K+]>CN(C)C=O.C(OCC)(=O)C.O>[CH2:1]([O:8][C:9]1[C:18]([O:19][CH3:33])=[C:17]2[C:12]([C:13](=[O:30])[C:14]([C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=3)=[C:15]([CH:20]([CH3:22])[CH3:21])[O:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 687027787-Benzyloxy-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one

생성물 1

HCID 687032587-Benzyloxy-3-(4-chlorophenyl)-2-isopropyl-8-methoxy-chromen-4-one

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 7-benzyloxy-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one (3.01 g, 7.15 mmol) and iodomethane (1.17 g, 8.22 mmol) in N,N-dimethylformamide (60 ml) is added K2CO3 (1.98 g, 14.3 mmol). The reaction mixture is stirred at room temperature for 72 h. The mixture is diluted with ethyl acetate and water, and the organic phase is washed with sodium thiosulfate solution and brine, dried (MgSO4) and concentrated in vacuo. The resulting off-white solid residue is triturated with ethyl acetate to afford the title compound as a white solid.

후처리

  1. washthe organic phase is washed with sodium thiosulfate solution and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe resulting off-white solid residue is triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-e8fed43ffcc74153aae0b172cb781dc4
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07732435B2

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