反应详情

温度

25 °C

The 4,8-dichloro compound from Example 250 (0.8 grams) was added to a solution of HOBT (1.2 grams) and sodium hydride (0.14 grams, 60% in mineral oil) in anhydrous dimethyl-formamide (60 mL). The resulting solution was irradiated with a 200 W lamp while stirring at 25° C. for 60 hours. The solution was poured into 1N aqueous NaOH while stirring and an additional 400 mL of water was added to the resulting mixture. Filtration provided a solid which was washed with water several times. The solid was dissolved in CH2Cl2 -acetone, dried over anhydrous MgSO4, and concentrated in vacuo to proved the title compound (0.87 grams, 90%, mp=120°-122° C., MH+ 563).

1. customThe resulting solution was irradiated with a 200 W lamp
2. stirringwhile stirring
3. filtrationFiltration
4. customprovided a solid which
5. washwas washed with water several times
6. dissolutionThe solid was dissolved in CH2Cl2 -acetone
7. dry with materialdried over anhydrous MgSO4
8. concentrationconcentrated in vacuo