反应详情

To a mixture of EXAMPLE 144B (8.3 g) was added water (75 mL) and H2SO4 (25 mL). The mixture was stirred at 0° C. while NaNO2 (3.13 g) in water (30 mL) was added. After stirring for 1 hour, the mixture was added to CuBr (5.45 g) in 48% HBr (200 mL). This mixture was stirred at 60° C. for 3 hours, cooled to room temperature, and partitioned between water and ethyl acetate. The organic layer was washed with aqueous Na2CO3 and dried (Na2SO4), filtered and concentrated.

1. additionwas added
2. stirringThis mixture was stirred at 60° C. for 3 hours
3. custompartitioned between water and ethyl acetate
4. washThe organic layer was washed with aqueous Na2CO3
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated