反应详情

Allantoin (1.58 g) was stirred with meta-iodobenzyl bromide (2.97 g) in DMF (25 ml) at 21° under nitrogen and sodium hydride (60% oil dispersion; 0.40 g) was added over 5 min. After 2 h the solution was partitioned between EtOAc and water and hydrochloric acid was added to give pH 3. The separated aqueous layer was extracted with more EtOAc and the combined organic layers were washed with water and brine twice. After drying (MgSO4), the solution was concentrated to 20 ml. After 1 h the solid was collected by filtration and washed with EtOAc. The residue was boiled with EtOAc (50 ml) and the slurry was allowed to cool. The solid was collected by filtration, washed with ethyl acetate and dried to give the title compound (0.507 g). LCMS RT=2.44 min

1. customAfter 2 h the solution was partitioned between EtOAc and water and hydrochloric acid
2. additionwas added
3. customto give pH 3
4. extractionThe separated aqueous layer was extracted with more EtOAc
5. washthe combined organic layers were washed with water and brine twice
6. dry with materialAfter drying (MgSO4)
7. concentrationthe solution was concentrated to 20 ml
8. filtrationAfter 1 h the solid was collected by filtration
9. washwashed with EtOAc
10. temperatureto cool
11. filtrationThe solid was collected by filtration
12. washwashed with ethyl acetate
13. customdried