反应详情

温度

140 °C

Sodium 2-methylpropan-2-olate (0.100 g, 1.06 mmol) was combined with compound 77 (0.150 g, 0.354 mmol) and tert-butyl 1-piperazinecarboxylate (0.099 g, 0.532 mmol) in 1,4-dioxane (3 ml). Nitrogen was bubbled through the solution for 1 min before adding XANTPHOS (0.031 g, 0.053 mmol) and Pd2(dba)3 (0.024 g, 0.026 mmol). The reaction mixture 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 over MgSO4 and concentrated in vacuum. The crude product was purified by flash column chromatography, eluting with a gradient of DCM-7% methanol/DCM to provide compound 78 as a brown oil (100 mg). LCMS-ESI (POS), M/Z, M+1: Found 529.3.

1. customNitrogen was bubbled through the solution for 1 min
2. custommicrowave irradiation for 1 hour
3. extractionextracted with 10% isopropanol/DCM
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated in vacuum
6. customThe crude product was purified by flash column chromatography
7. washeluting with a gradient of DCM-7% methanol/DCM