Sodium Thiosulfate → 6-Methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine

HRID 1862312Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1862312
Cl[C:2]1C=C(C=CC=1)C(OO)=O.[CH3:12][O:13][C:14]1[N:19]=[C:18](SC)[N:17]=[C:16]([O:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])[CH:15]=1.[S:28]([O-:32])([O-])(=[O:30])=S.[Na+].[Na+].C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[CH3:12][O:13][C:14]1[N:19]=[C:18]([S:28]([CH3:2])(=[O:32])=[O:30])[N:17]=[C:16]([O:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])[CH:15]=1

Komponenten

6

Edukt 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 186191496-Methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine

Produkt 1

HCID 186191946-Methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

2.59 g of 3-chloroperoxybenzoic acid was added to a solution of 1.22 g of 6-methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine in 10 ml of chloroform at 0° C. The mixture was stirred at room temperature for 3 hours, then 30 ml of saturated aqueous sodium thiosulfate solution was added to the mixture. The mixture was poured into saturated aqueous sodium bicarbonate solution, extracted with chloroform, the organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated, then, the resulted residue was subjected to silica gel chromatography to obtain 1.32 g of 6-methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washthe organic layer was washed with saturated saline
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-56687f8b62bf45dd94a4930e2edc09c4
Quelldatensatz
uspto-grants-2003_03
Patentnummer
US06537948B1

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