反应详情

温度

0 °C

Sodium hydride (60% dispersion in mineral oil, 0.205 g, 5.13 mmol) was suspended in 5 mL dimethylformamide. The mixture was stirred for 10 min and then cooled at 0° C. with an ice bath. 5-Bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidine (1 g, 4.30 mmol) dissolved in 5 mL dimethylformamide was added dropwise and the mixture was stirred for 30 min. At the same temperature [2-(chloromethoxy)ethyl](trimethyl)silane (0.9 g, 5.4 mmol) dissolved in 5 mL dimethylformamide was added dropwise and stirred for 30 min at 0° C. The mixture was poured into water and extracted twice with ethyl acetate. The organics were dried over sodium sulphate and concentrated under reduced pressure. The residue was purified using SP1® Purification System (0% to 100%, hexane-ethyl acetate) to give 1.18 g (76% yield) of the title compound as a white solid. Purity 100%.

1. additionwas added dropwise
2. stirringthe mixture was stirred for 30 min
3. additionwas added dropwise
4. stirringstirred for 30 min at 0° C
5. extractionextracted twice with ethyl acetate
6. dry with materialThe organics were dried over sodium sulphate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified
9. customSP1® Purification System (0% to 100%, hexane-ethyl acetate)