m-Chloroperbenzoic acid → Methyl 3-fluoro-2-methylsulphonylbenzoate

HRID 1491581ノート

反応式

HRID 1491581 の反応式
[F:1][C:2]1[C:3](SC)=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].Cl[C:15]1C=CC=C(C(OO)=O)C=1.[S:25](S([O-])=O)([O-:28])(=O)=[O:26].[Na+].[Na+]>ClCCl>[F:1][C:2]1[C:3]([S:25]([CH3:15])(=[O:28])=[O:26])=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6]

参加物

5

反応物 3

HCID 70297m-Chloroperbenzoic acidHCID 656671Sodium PyrosulfiteHCID 18953297Methyl 3-fluoro-2-(methylthio)benzoate

生成物 1

HCID 18953324Methyl 3-fluoro-2-methylsulphonylbenzoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

A mixture of methyl 3-fluoro-2-methylsulphenylbenzoate (14.0 g) and 3-chloroperbenzoic acid (50-60%, 55.0 g) in dichloromethane was stirred at 25° C. for 1.5 hours. 1M Sodium metabisulphite was added and the organic phase washed with sodium bicarbonate and brine, dried over sodium sulphate, filtered and evaporated. The product was recrystallised from ethyl acetate to give 8.6 g of methyl 3-fluoro-2-methylsulphonylbenzoate as white crystals, m.p. 116.2° C.

後処理

  1. washthe organic phase washed with sodium bicarbonate and brine
  2. dry with materialdried over sodium sulphate
  3. filtrationfiltered
  4. customevaporated
  5. customThe product was recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-97a009b276364dcc8a1f7d05e2ee5542
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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