反应详情

温度

0 °C

To 935 mg 2,4-dichloro-7H-pyrrolo[2,3-d]pyrimidine (3a) (5.0 mmol) in 100 mL of 1,4-dioxane was slowly added 256 μL of Br2 (5.0 mmol) at 0° C. over a period of 10 minutes. After stirring for 30 minutes at 0° C., the reaction mixture was poured into a mixture of 150 mL of EtOAc and 150 mL of saturated aqueous Na2SO3 then filtered through celite. The aqueous phase was extracted with EtOAc (3×100 mL) and combined organic layers were washed with brine, concentrated and purified by flash column chromatography to give the title compound.

1. customat 0° C.
2. customof 10 minutes
3. filtrationthen filtered through celite
4. extractionThe aqueous phase was extracted with EtOAc (3×100 mL)
5. washwere washed with brine
6. concentrationconcentrated
7. custompurified by flash column chromatography