Pyridine → HCID 19860691, Verbindung

HRID 2413849Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2413849
[F:1][C:2]([F:8])([CH2:5][CH2:6][OH:7])[CH2:3][OH:4].N1C=CC=CC=1.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>ClCCl>[CH3:15][S:16]([O:4][CH2:3][C:2]([F:8])([F:1])[CH2:5][CH2:6][O:7][S:16]([CH3:15])(=[O:18])=[O:17])(=[O:18])=[O:17]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 13935577108781-20-0

Produkt 1

HCID 19860691HCID 19860691, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred mixture of 2,2-difluoro-1,4-butanediol (12.97 g, 103 mM), dry pyridine (65 mL) and dichloromethane (200 mL), is slowly added a solution of methanesulfonyl chloride (23.6 g) in dichloromethane (50 mL). Stirring is continued overnight, and the mixture is washed with 2N HCl (twice), 10% aqueous NaHCO3 until neutral, and finally with water. The organic solution is dried (MgSO4) and evaporated to yield 1,4-bis-methanesulfonyloxy-2,2-difluorobutane as a slightly yellow oil (25.4 g, 87.5%) which crystallizes on scratching with dry ether: white crystals, 22.3 g (77%).

Aufarbeitung

  1. washthe mixture is washed with 2N HCl (twice), 10% aqueous NaHCO3 until neutral, and finally with water
  2. dry with materialThe organic solution is dried (MgSO4)
  3. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f48a691379d84dec80926be71d5f74f5
Quelldatensatz
uspto-grants-1988_01
Patentnummer
US04719313

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