Water → Methyl 2-methylsulphonyl-3-phenylsulphenylbenzoate

HRID 1491580ノート

反応式

HRID 1491580 の反応式
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]

参加物

7

反応物 4

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

生成物 1

HCID 18953302Methyl 2-methylsulphonyl-3-phenylsulphenylbenzoate収率 46.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09af85754802491ebebb86024e751be8
出典データセット
uspto-grants-1994_12
特許番号
US05371064

反応ノート

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