反应详情

温度

140 °C

Sodium 2-methylpropan-2-olate (0.142 g, 1.48 mmol) was combined with compound 4 (0.125 g, 0.493 mmol) and 2,5-dibromo-3-methylpyridine (0.149 g, 0.592 mmol) in 1,4-dioxane (3 ml). The reaction mixture was degassed by bubbling nitrogen through the solution for ˜1 mM, followed by the addition of XANTPHOS (0.0428 g, 0.0740 mmol) and Pd2(dba)3 (0.0339 g, 0.0370 mmol). The reaction was heated to 140° C. using microwave irradiation for 1 hour. The reaction mixture was poured into sat. NH4Cl and extracted with 10% isopropanol/DCM. The organic layer was dried with MgSO4 and concentrated in vacuum. Purification by flash column chromatography, eluting with a gradient of DCM-5% methanol/DCM provided compound 77 as a yellow solid (150 mg, 71%). LCMS-ESI (POS), M/Z, M+1: Found 423.1

1. customThe reaction mixture was degassed
2. customby bubbling nitrogen through the solution for ˜1 mM
3. custommicrowave irradiation for 1 hour
4. extractionextracted with 10% isopropanol/DCM
5. dry with materialThe organic layer was dried with MgSO4
6. concentrationconcentrated in vacuum
7. customPurification by flash column chromatography
8. washeluting with a gradient of DCM-5% methanol/DCM provided compound 77 as a yellow solid (150 mg, 71%)