反应详情

A mixture of 1-isopropyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (117.1 mg, 0.4958 mmol), methyl 10-iodo-6,7-dihydroimidazo[1,2-d]pyrido[3,2-b][1,4]oxazepine-3-carboxylate (92.0 mg, 0.248 mmol), [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1) (20.24 mg, 0.02479 mmol) and 1.0 M of Potassium acetate in water (0.49 mL) in 1,2-Dimethoxyethane (5.0 mL, 48 mmol) was degassed. The reaction was microwaved on 200 watts, 140° C. for 40 minutes. The reaction mixture was filtered, washed with DME, mixed with water and extracted with EtOAc. Combined organic extracts were washed with 1% aq NaOH to remove a phenolic byproduct, then 5% aq citric acid, water, brine, dried over Na2SO4 and concentrated in vacuum. The residue was purified on 4 g silica column, eluting with 60-70% of EtOAc in heptane. Yield 21 mg. MS (ESI+): 354.2.

1. customwas degassed
2. customThe reaction was microwaved on 200 watts, 140° C. for 40 minutes
3. filtrationThe reaction mixture was filtered
4. washwashed with DME
5. additionmixed with water
6. extractionextracted with EtOAc
7. washCombined organic extracts were washed with 1% aq NaOH
8. customto remove a phenolic byproduct
9. dry with material5% aq citric acid, water, brine, dried over Na2SO4
10. concentrationconcentrated in vacuum
11. customThe residue was purified on 4 g silica column
12. washeluting with 60-70% of EtOAc in heptane