反应详情

温度

65 °C

6-cyclopropyl-2-(methylsulfonyl)pyrimidine-4-carboxylic acid (I-20A). Into a 40 mL vessel was added 6-cyclopropyl-2-(methylthio)pyrimidine-4-carboxylic acid_(commerically available, Enamine Ltd, catalog number EN300-422464, 250 mg, 1.19 mmol) and acetonitrile (12.5 mL). This resulting solution was then added dropwise at RT over 5 min. to a separate 40 mL reaction vessel that was charged with a rapidly stirred suspension of Oxone™ (using Aldrich supplied Oxone which is a multicomponent triple salt mixture containing potassium monopersulfate, 2 KHSOs5.KHSO4.K2SO4, 2.50 g, 4.10 mmol) and water (15 mL). Upon complete addition of the methyl thiopyrimidine, the resulting suspension was heated to 65° C. for 20 min. and subsequently cooled to RT. The resulting yellow suspension was extracted with ethyl acetate (4×100 mL) and the organic extracts were dried over magnesium sulfate, filtered and concentrated to furnish the methyl sulfonyl pyrimidine as a residue that was used directly in the next step without isolation. MS m/z 243.1 (M+1).

1. additionThis resulting solution was then added dropwise at RT over 5 min. to a separate 40 mL reaction vessel that
2. temperaturesubsequently cooled to RT
3. extractionThe resulting yellow suspension was extracted with ethyl acetate (4×100 mL)
4. dry with materialthe organic extracts were dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated