反应详情

To a suspension of 2-amino-4-methyl-5-(4-methylpyridin-2-yl)-thiazole and 2-(methylthio)-2-thiazoline (127 mg) in methoxyethanol (2 ml) was added a solution of hydrogen chloride in 1,4-dioxane (4N, 0.23 ml). The mixture was refluxed for 20 hours, poured into a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate twice. The combined organic layer was washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, 5% methanol in dichloromethane) and recrystallized from chloroform (1 ml)-diisopropyl ether (3 ml) to give 2-(4-methyl-5-(4-methylpyridin-2-yl)thiazol-2-ylamino)-2-thiazoline (110 mg).

1. temperatureThe mixture was refluxed for 20 hours
2. extractionextracted with ethyl acetate twice
3. washThe combined organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography (silica gel 25 g, 5% methanol in dichloromethane)
7. customrecrystallized from chloroform (1 ml)-diisopropyl ether (3 ml)