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

HRID 1491581Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1491581
[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]

Komponenten

5

Edukt 3

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

Produkt 1

HCID 18953324Methyl 3-fluoro-2-methylsulphonylbenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-97a009b276364dcc8a1f7d05e2ee5542
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05371064

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