反应详情

温度

45 °C

In a 12 mL septum capped vial purged with N2 add N-[4-(7-chloro-imidazo[1,2-a]pyridin-3-yl)-benzyl]-2-(m-trifluoromethyl-phenyl)-acetamide (144 mg, 0.32 mmol), 4-(methylsulfonyl)phenyl boronic acid (89 mg, 0.44 mmols), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (23.6 mg) [X-Phos is alternatively used as the ligand in this reaction], Pd(OAc)2 (6 mg), K3PO4 (218 mg, 1.02 mmol), 1,4-dioxane: H2O 2:1 (5 mL). Deoxygenate the vial again with N2 then heat to 45° C. for 24 hours. Cool the reaction and transfer to a separatory funnel and discard the bottom aqueous layer. Evaporate the solvents under vacuum and take up the residue into CH2Cl2 with a trace of MeOH. Chromatograph the crude reaction on SiO2 eluting with a gradient of 0% to 8% of 2 M NH3 in MeOH with the balance CH2Cl2 Dry the product in a vacuum oven at 40° C. for 24 hours to give 38.6 mg (21%) MS (ES), m/z 564.3 (M+1).

1. custompurged with N2
2. customDeoxygenate the vial again with N2
3. temperatureCool
4. customthe reaction and transfer to a separatory funnel
5. customEvaporate the solvents under vacuum
6. customChromatograph the crude reaction on SiO2 eluting with a gradient of 0% to 8% of 2 M NH3 in MeOH with the balance CH2Cl2
7. customDry the product in a vacuum oven at 40° C. for 24 hours
8. customto give 38.6 mg (21%)