反应详情

温度

100 °C

A mixture of 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene -2-carboxamide (100 mg, 0.45 mmol), 8-phenyl-1,4-dioxa-8-azaspiro[4.5]decane (109 mg, 0.50 mmol), CSA (125 mg, 0.54 mmol), MgSO4 (108 mg, 0.90 mmol) and DMA (1 mL) was stirred at 100° C. for 1 h. Then, saturated aqueous NaHCO3 was added to quench the reaction. The organic materials were extracted with EtOAc/THF. The combined extracts were dried over Na2SO4 and filtered. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, NH, 80:20 hexane/EtOAc to EtOAc then to 95:5 EtOAc/MeOH), then crystallized from MeOH/EtOAc/heptane to give the title compound (46 mg, 27%) as a yellow solid:

1. customto quench
2. customthe reaction
3. extractionThe organic materials were extracted with EtOAc/THF
4. dry with materialThe combined extracts were dried over Na2SO4
5. filtrationfiltered
6. customAfter removal of the solvent at reduced pressure
7. customthe residue was purified by column chromatography (Purif, NH, 80:20 hexane/EtOAc to EtOAc
8. customto 95:5 EtOAc/MeOH), then crystallized from MeOH/EtOAc/heptane