反应详情

To a stirred solution of 1-(4-cyano-3-fluorophenyl)-1-[1-(triphenylmethyl)imidazol-4-yl]ethanol, as described above in Step C, (200 mg, 0.42 mmol), methyl glycolate (35 mg, 0.39 mmol), and N,N-diisopropylethylamine (65 mg, 0.51 mmol) in dry CH2Cl2 (10 mL), under argon, at −78° C., was added trifluoromethanesulfonic anhydride (110 mg, 0.39 mmol) dropwise. The mixture was allowed to warm slowly to ambient temperature, then the solvent was removed in vacuo. The residue was dissolved in MeOH (10 mL) and the solution was heated to reflux for 1 hour, then concentrated to dryness. The residue was purified by silica gel chromatography, eluting with 4% MeOH—0.4% NH4OH in CHCl3, to yield the titled product as a white solid.

1. customthe solvent was removed in vacuo
2. dissolutionThe residue was dissolved in MeOH (10 mL)
3. temperaturethe solution was heated
4. temperatureto reflux for 1 hour
5. concentrationconcentrated to dryness
6. customThe residue was purified by silica gel chromatography
7. washeluting with 4% MeOH—0.4% NH4OH in CHCl3