反应详情

温度

-78 °C

2.5 M n-Butyllithium in hexane (0.860 mL) was added dropwise to a −78° C. solution of 4-(1,3-thiazol-5-yl)-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidine (550 mg, 0.0016 mol) in THF (20 mL). The mixture was stirred for 30 minutes at −78° C., followed by the slow addition of carbon tetrabromide (658 mg, 0.00198 mol) as a solution in THF (10 mL). After 30 minutes, the mixture was quenched with a small amount of saturated ammonium chloride, diluted with ether, and dried over sodium sulfate. The residue obtained after filtration and concentration was purified by flash column chromatography (ethyl acetate/hexanes) to afford the desired product (387 mg, 57%).

1. waitAfter 30 minutes
2. customthe mixture was quenched with a small amount of saturated ammonium chloride
3. additiondiluted with ether
4. dry with materialdried over sodium sulfate
5. customThe residue obtained
6. filtrationafter filtration and concentration
7. customwas purified by flash column chromatography (ethyl acetate/hexanes)