反应详情

温度

115 °C

In a 15 mL microwave reaction vial was added potassium phosphate tribasic (1.43 g, 6.74 mmol), 6-bromopyridazin-3-amine (335 mg, 1.93 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,6-tetrahydropyridinium chloride (500 mg, 1.93 mmol), X-PHOS (138 mg, 289 μmol) and bis(dibenzylideneacetone)palladium (83 mg, 144 μmol) in 7 mL n-butanol and 1.4 mL H2O. The tube was sealed under argon and heated at 115° C. in oil bath for 3 hrs then stirred at room temperature overnight. The phases were separated and the aqueous was extracted with EtOAc. (10 ml). Water (20 mL) was added to the residual aqueous phase and was extracted with DCM (3×10 mL). The extracts were combined with the EtOAc organic phase. The resultant solution was absorbed onto silica gel and purified by LC chromatography eluting with 0-10% (10% NH4OH in MeOH) in 1/1 EtOAc/hexane to afford 300 mg (82%) of the title compound.

1. customIn a 15 mL microwave reaction
2. customThe tube was sealed under argon
3. customThe phases were separated
4. extractionthe aqueous was extracted with EtOAc
5. additionWater (20 mL) was added to the residual aqueous phase
6. extractionwas extracted with DCM (3×10 mL)
7. customThe resultant solution was absorbed onto silica gel
8. custompurified by LC chromatography
9. washeluting with 0-10% (10% NH4OH in MeOH) in 1/1 EtOAc/hexane