反应详情

温度

23 °C

To a suspension of 8-[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-1,4-dioxaspiro[4.5]decane-8-carboxamide (700 mg, 1.35 mmol) in anhydrous THF (2 ml) and was added concentrated HCl (5.53 ml, 67.4 mmol). The resulting dark yellow solution was stirred at 23° C. for 6 h. The mixture was diluted with saturated aqueous NaHCO3 (80 ml) and extracted with EtOAc (2×70 ml). The combined organic layers were dried over Na2SO4, filtered and concentrated. The crude oil was triturated with hexanes and diethyl ether which afforded 1-[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-4-oxocyclohexanecarboxamide (683 mg, 1.01 mmol, 74.6%) as an tan solid. MS APCI: [M+H]+ m/z 476.1.

1. extractionextracted with EtOAc (2×70 ml)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude oil was triturated with hexanes and diethyl ether which