Reaktion #1004559

Reaktionsgleichung

m-chloroperbenzoic acid

4,4-difluoro-3-methyl-3-butenyl 4-methyl-2-(methylthio)pyrimidine-5-carboxylate

sodium hydrogensulfite

→

4,4-difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate

Ausbeute 92.0%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   Temperaturcooling
3. 3
   Filtrationthe mixture was filtered
4. 4
   WaschenThe organic layer was washed with a saturated sodium hydrogencarbonate solution and water in this order
5. 5
   Trocknenby drying over anhydrous magnesium sulfate
6. 6
   workup.ADDITIONthe addition of “Florisil”
7. 7
   Filtrationfiltering
8. 8
   EinengenThe solution was concentrated at 40° C. under reduced pressure

Vorschrift

To 20 ml of chloroform was dissolved 1.10 g (3.8 mmol) of 4,4-difluoro-3-methyl-3-butenyl 4-methyl-2-(methylthio)pyrimidine-5-carboxylate, followed by the addition, in three portions, of 2.00 g (8.1 mmol) of 70% m-chloroperbenzoic acid under ice-cooling and stirring for 1 hour after warming to room temperature. An aqueous solution of sodium hydrogensulfite was added under ice-cooling and the mixture was filtered to fractionate an organic layer. The organic layer was washed with a saturated sodium hydrogencarbonate solution and water in this order, followed by drying over anhydrous magnesium sulfate, the addition of “Florisil” and filtering. The solution was concentrated at 40° C. under reduced pressure to obtain 1.13 g (yield: 92%) of 4,4-difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate.

Quelle