Water → Methyl 2-methylsulphonyl-3-phenylsulphenylbenzoate

HRID 1491580노트

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HRID 1491580 반응식
F[C:2]1[C:3]([S:12]([CH3:15])(=[O:14])=[O:13])=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].C(=O)([O-])[O-].[K+].[K+].[C:22]1([SH:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.O>CN(C)C=O.C(OCC)(=O)C>[CH3:15][S:12]([C:3]1[C:2]([S:28][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[CH:11][CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6])(=[O:14])=[O:13]

참가 물질

7

반응물 4

HCID 962WaterHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 18953324Methyl 3-fluoro-2-methylsulphonylbenzoate

생성물 1

HCID 18953302Methyl 2-methylsulphonyl-3-phenylsulphenylbenzoate수율 46.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

A mixture of methyl 3-fluoro-2-methylsulphonylbenzoate (10.9 g), potassium carbonate (7.8 g) and thiophenol (5.4 g) in N,N-dimethylformamide was stirred at 25° C. for six hours. Water and ethyl acetate were added and the resulting solid collected by filtration and combined with the solid obtained from washing the organic phase of the flitrate with brine, drying over magnesium sulphate, filtering and evaporating. This product was recrystallised from ethyl acetate to give 7.0 g of methyl 2-methylsulphonyl-3-phenylsulphenylbenzoate as white crystals, mp 151.1° C.

후처리

  1. filtrationthe resulting solid collected by filtration
  2. customobtained
  3. washfrom washing the organic phase of the flitrate with brine
  4. dry with materialdrying over magnesium sulphate
  5. filtrationfiltering
  6. customevaporating
  7. customThis product was recrystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-09af85754802491ebebb86024e751be8
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371064

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