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Methyl iodide → 4-methoxy-4'-methylbiphenyl-3-yl-phosphonic Acid Dimethyl Ester

HRID 1018972
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HRID 1018972 반응식
[CH3:1][O:2][P:3]([C:7]1[CH:8]=[C:9]([C:14]2[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=2)[CH:10]=[CH:11][C:12]=1[OH:13])(=[O:6])[O:4][CH3:5].I[CH3:22].[OH-].[Na+]>CN(C=O)C>[CH3:1][O:2][P:3]([C:7]1[CH:8]=[C:9]([C:14]2[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=2)[CH:10]=[CH:11][C:12]=1[O:13][CH3:22])(=[O:6])[O:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 18342343HCID 18342343, 화합물

생성물 1

HCID 599208424-methoxy-4'-methylbiphenyl-3-yl-phosphonic Acid Dimethyl Ester수율 63.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-hydroxy-4′-methylbiphenyl-3-yl-phosphonic acid dimethyl ester (500 mg, 1.7 mmol), iodomethane (342 mg, 2.4 mmol) and 10 M aqueous NaOH (190 μL, 1.9 mmol) in DMF (10 mL) was stirred at r.t. overnight. After dilution with H2O, the mixture was extracted with EtOAc. Chromatography over silica gel and elution with EtOAc with 5% of MeOH gave 330 mg (63%) of title compound as a white solid.

후처리

  1. extractionAfter dilution with H2O, the mixture was extracted with EtOAc
  2. washChromatography over silica gel and elution with EtOAc with 5% of MeOH

출처 및 근거

ORD 기록
ord-35eb466e164b479ea2fc4897e87333b5
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06486141B2

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