反应详情

温度

-35 °C

To a stirred solution of 5-bromo-2,4-dichloropyrimidine (Aldrich, 454 mg, 2 mmol) in THF at −78° C., diisopropyl magnesium chloride (2M solution in THF, 2.1 mmol, 1.05 mL) was added and the mixture was stirred for 30 minutes at −35° C. Next, the solution was cooled to −78° C. and 1 mL of dry DMF was added. The mixture was stirred for 120 minutes at −78° C. and the reaction was quenched with 1 N HCl. The mixture was extracted with EtOAc and dried with sodium sulfate. The solvent was removed and the residue was chromatographed to give a brown solid. 102 mg, 28%. H1NMR (CDCl3), δ (ppm), 9.0 (s, 1 H), 10.4 (s, 1 H).

1. temperatureNext, the solution was cooled to −78° C.
2. stirringThe mixture was stirred for 120 minutes at −78° C.
3. customthe reaction was quenched with 1 N HCl
4. extractionThe mixture was extracted with EtOAc
5. dry with materialdried with sodium sulfate
6. customThe solvent was removed
7. customthe residue was chromatographed
8. customto give a brown solid