反应详情

12.1 g (about 39.65 mmol) of the compound from Example 6A were initially charged in DMF (217 ml), and 8.25 g (43.62 mmol) of 2-fluorobenzyl bromide and 14.21 g (43.62 mmol) of caesium carbonate were then added. The mixture was stirred at RT for two hours. The reaction mixture was then added to water (1.17 l) and extracted twice with ethyl acetate (502 ml). The collected organic phases were washed with saturated aqueous sodium chloride solution (335 ml), dried, filtered and concentrated. The residue was chromatographed on silica gel (mobile phase:petroleum ether/ethyl acetate 97:3) and the product fractions were concentrated. This gave 9.0 g (61% of theory) of the title compound as a solid. The solid was taken up in ethyl acetate and washed with 10% strength aqueous sodium thiosulphate solution and then with saturated aqueous sodium chloride solution, dried and concentrated.

1. extractionextracted twice with ethyl acetate (502 ml)
2. washThe collected organic phases were washed with saturated aqueous sodium chloride solution (335 ml)
3. customdried
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel (mobile phase:petroleum ether/ethyl acetate 97:3)
7. concentrationthe product fractions were concentrated
8. washwashed with 10% strength aqueous sodium thiosulphate solution
9. dry with materialwith saturated aqueous sodium chloride solution, dried
10. concentrationconcentrated