Reaktionsgleichung
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:3]=1[CH2:4][S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1.ClC1C=CC=C(C(OO)=[O:25])C=1.[OH2:28]>C(Cl)(Cl)Cl>[CH3:1][C:2]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:3]=1[CH2:4][S:5]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1)(=[O:25])=[O:28]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a well-stirred and cooled (−10° C.) solution of 6.9 g (0.03 mole) of 2-(2,5-dimethyl-benzylthio)pyridine in 75 ml of chloroform was added portion-wise a solution of 12 g (0.06 mole) of metachloroperbenzoic acid dissolved in 100 ml of chloroform. The mixture was kept at −10° C. for 10 minutes and then allowed to warm to room temperature over the next six hours. It was stirred at room temperature overnight. Water was then added and the phases separated. he chloroform phase was washed with aqueous sodium bicarbonate and then again with water. he chloroform phase was dried with anhydrous sodium sulfate, filtered, and the chloroform removed using a rotary evaporator to give 8 g of an oil. The oil was crystallized from a small amount of ethanol, with a melting point of 77-78° C., and a yield of 3 g (30%). IR spectrum showed the presence of SO2 at 1160, 1310 cm−1.
Aufarbeitung
- stirringIt was stirred at room temperature overnight
- customthe phases separated
- washhe chloroform phase was washed with aqueous sodium bicarbonate
- dry with materialhe chloroform phase was dried with anhydrous sodium sulfate
- filtrationfiltered
- customthe chloroform removed
- customa rotary evaporator
Quellen und Nachweise
- ORD-Eintrag
- ord-68f1ae8e5be1470bb31639fdb16b0fa7
- Quelldatensatz
- uspto-grants-2002_12
- Patentnummer
- US06498254B1
Verknüpfte Notizen
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