反应详情

温度

120 °C

Degas a mixture of 1-bromo-2-(2-bromo-6-fluoro-benzyloxy)-4-fluoro-benzene (886 mmol, 335 g), ethyl acrylate (931 mmol, 101 mL, 1.05 eq), Pd(OAc)2 (22.2 mmol, 4.97 g), tetrabutylammonium bromide (886 mmol, 286 g), and sodium acetate (4.40 mol, 363.5 g) in N-methylpyrrolidinone (3.3 L) by evacuating and back-filling with nitrogen five times. Heat the mixture to 120° C. for 2 h. Cool to 35° C. and add water (5.5 L) over 40 min. Filter the precipitate, rinse with water (2×500 mL) and air dry for 30 min. Reslurry the in isopropanol (1 L) for 2 h and cool on ice for one hour. Collect the dark gray solid by filtration, rinse with cold isopropanol (5×100 mL) and dry at 50° C. in vacuo to obtain the title compound (191 g, 68%).

1. customDegas
2. customby evacuating and back-filling with nitrogen five times
3. temperatureCool to 35° C.
4. additionadd water (5.5 L) over 40 min
5. filtrationFilter the precipitate
6. washrinse with water (2×500 mL) and air
7. customdry for 30 min
8. customfor 2 h
9. temperaturecool on ice for one hour
10. customCollect the dark gray solid
11. filtrationby filtration
12. washrinse with cold isopropanol (5×100 mL)
13. customdry at 50° C. in vacuo