反应详情

A 1 M toluene solution of 5.87 ml (5.87 mmol) of (cyanomethylene)tributylphosphorane was added to a solution of 2.22 g (3.91 mmol) of the title compound produced in step (ii) of Reference Example 12 in toluene (55.0 ml), and the mixture was stirred with heating under reflux for 1 hr 20 min. The reaction solution was then cooled to room temperature, and the solvent was removed under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1) to give 1.16 g (yield 54%) of the title compound.

1. temperaturewith heating
2. temperatureunder reflux for 1 hr 20 min
3. customthe solvent was removed under the reduced pressure
4. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1)