反应详情

A mixture of 6-bromo-3-[(4-methyl-1-piperazinyl)methyl]-1,2-benzisoxazole (Intermediate 46) (0.02 g) N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (Intermediate 5) (0.02 g) 2N aqueous sodium carbonate and tetrakis(triphenylphosphine)palladium(0) (1 mg) in isopropanol (0.3 ml) was heated in a Reactivial™ at 65° for 18 h. the reaction mixture was partitioned between water and ethyl acetate, the phases were separated and the aqueous layer was re-extracted with ethyl acetate. The combined organic extracts were washed with water (×2) and brine, dried using a hydrophobic filter tube and concentrated under a stream of nitrogen. The residue was purified by reverse phase preparative Hplc to give the title compound as a white foam (0.006 g).

1. temperaturewas heated in a Reactivial™ at 65° for 18 h. the reaction mixture
2. customwas partitioned between water and ethyl acetate
3. customthe phases were separated
4. extractionthe aqueous layer was re-extracted with ethyl acetate
5. washThe combined organic extracts were washed with water (×2) and brine
6. customdried
7. concentrationconcentrated under a stream of nitrogen
8. customThe residue was purified by reverse phase preparative Hplc