反应详情

温度

80 °C

tert-Butyl 5-(tert-butyldiphenylsilanyloxy)-3-[5-iodo-1-(3-isobutylcyclobutyl)-1H-[1,2,3]triazol-4-yl]valerate (340 mg), 2-cyclopropyl-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (0.16 mL), tripotassium phosphate (403 mg), N,N-dimethylacetamide (3.4 mL) and water (0.85 mL) were mixed. The mixture was degassed by bubbling argon gas. To the mixture was added PdCl2(PPh3)2 (50 mg). The mixture was stirred at 80° C. for 1 hr. To the reaction mixture was added ethyl acetate at ice temperature, and then the mixture was filtered. The filtrate was washed with water and brine, then dried over magnesium sulfate. The magnesium sulfate was filtered off and the filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/20) to give the title compound (238 mg).

1. customThe mixture was degassed
2. customby bubbling argon gas
3. additionTo the mixture was added PdCl2(PPh3)2 (50 mg)
4. additionTo the reaction mixture was added ethyl acetate at ice temperature
5. filtrationthe mixture was filtered
6. washThe filtrate was washed with water and brine
7. dry with materialdried over magnesium sulfate
8. filtrationThe magnesium sulfate was filtered off
9. concentrationthe filtrate was concentrated in vacuo
10. customThe resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/20)