反应详情

To a solution of the title compound of Step B (11.2 g) in acetone (400 mnL) was added an aqueous solution of 1N hydrochloric acid (6 mL) and the mixture was heated at reflux overnight. After cooling, the mixture was concentrated under reduced pressure and the resulting residue was dissolved in diethyl ether and dried (MgSO4). The drying agent was removed by filtration and the solvent was removed under reduced pressure to give a yellow oil. The crude product was combined with another batch of crude product prepared in the same manner and purified by distillation (47 Pa, 58-59° C.) to afford 8.9 g of the title compound of Step C as an oil. 1H NMR (CDCl3): δ 8.11 (s,1H), 7.92 (d,1H), 7.7 (d,1H), 7.47 (t,1H), 2.62 (s,3H), 0.30 (s,8H).

1. temperaturethe mixture was heated
2. temperatureat reflux overnight
3. temperatureAfter cooling
4. concentrationthe mixture was concentrated under reduced pressure
5. dissolutionthe resulting residue was dissolved in diethyl ether
6. dry with materialdried (MgSO4)
7. customThe drying agent was removed by filtration
8. customthe solvent was removed under reduced pressure
9. customto give a yellow oil
10. customprepared in the same manner
11. distillationpurified by distillation (47 Pa, 58-59° C.)