反应详情

200 mg (0.75 mmol) of methyl [3-(4-chlorophenyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]acetate [preparation according to WO 2007/134862 Example 222A] were suspended in 7.5 ml of acetone, 365 mg (1.12 mmol) of cesium carbonate and 223 mg (0.97 mmol) of methyl 3-bromomethylbenzoate were added and the mixture was heated at the boil for 1 h. After cooling, the mixture was filtered through Extrelut and the filter cake was rinsed with acetone. The filtrate was concentrated under reduced pressure and the residue was purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1→1:1). The target compound was obtained as a colorless foam (165 mg, 53% of theory).

1. temperaturethe mixture was heated at the boil for 1 h
2. temperatureAfter cooling
3. filtrationthe mixture was filtered through Extrelut
4. washthe filter cake was rinsed with acetone
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe residue was purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1→1:1)
7. customThe target compound was obtained as a colorless foam (165 mg, 53% of theory)