反应详情

A stirred mixture of 3-(4-chlorophenyl)-2-isopropyl-4-oxo-9,10-dihydro-4H,8H-1,11-dioxa-7-aza-cyclohepta[a]naphthalene-7-carbaldehyde (0.063 g, 0.158 mmol) in 1M HCl solution (4 ml) and methanol (6 ml) is heated under reflux for 1 h under a nitrogen atmosphere. The mixture is allowed to cool to room temperature, and the methanol solvent is removed by evaporation in vacuo. The concentrated mixture is diluted with water (5 ml) and treated with solid sodium hydrogen carbonate, until a pH of 7-8 is attained. The mixture is washed successively with ethyl acetate and methylene chloride. The combined organic phases are dried (magnesium sulfate) and filtered, and the solvent is removed by evaporation in vacuo to afford a crude orange solid. This is stirred overnight in a solution of 2M HCl in diethyl ether (3 ml), filtered and dried at room temperature under high vacuum to give the title compound as a cream-coloured solid.

1. temperatureis heated
2. temperatureunder reflux for 1 h under a nitrogen atmosphere
3. customthe methanol solvent is removed by evaporation in vacuo
4. additionThe concentrated mixture is diluted with water (5 ml)
5. additiontreated with solid sodium hydrogen carbonate, until a pH of 7-8
6. washThe mixture is washed successively with ethyl acetate and methylene chloride
7. dry with materialThe combined organic phases are dried (magnesium sulfate)
8. filtrationfiltered
9. customthe solvent is removed by evaporation in vacuo
10. customto afford a crude orange solid
11. filtrationfiltered
12. customdried at room temperature under high vacuum