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

HRID 1491581노트

반응식

HRID 1491581 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18953324Methyl 3-fluoro-2-methylsulphonylbenzoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-97a009b276364dcc8a1f7d05e2ee5542
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371064

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