反应详情

温度

0 °C

Under argon atmosphere, 2.5 mL of bromotrimethylsilane is added to a solution of 0.80 g of (S)-[1-(4-cyano-3-trifluoromethylphenyl)-2,5-dioxo-3-methyl-4-phenylimidazolidin-4-yl]methyl diethyl phosphate in 25 mL of DCM cooled at 0° C. The reaction is stirred for 1 hour at 0° C. then 18 hours at room temperature. The solvent is evaporated then the residue is dissolved in a mixture of water and methanol. Solvents are evaporated and this process repeated twice. The crude product is purified by chromatography over silica gel while eluting with 90/10/1/1 to 85/15/2/2 dichloromethane/methanol/acetic acid/water mixture to provide the desired compound.

1. custom18 hours
2. customat room temperature
3. customThe solvent is evaporated
4. dissolutionthe residue is dissolved in a mixture of water and methanol
5. customSolvents are evaporated
6. customThe crude product is purified by chromatography over silica gel
7. washwhile eluting with 90/10/1/1 to 85/15/2/2 dichloromethane/methanol/acetic acid/water mixture