反应详情

P-Nitroacetophenone (1.65 g, 10 mmol), ethylene glycol (5 ml, 89 mmol), triethyl orthoformate (2.96 g, 20 mmol), and p-toluenesulfonic acid (0.086 g, 0.5 mmol) were combined in methylene chloride (4 ml). The solution was heated with an oil bath (50°-70° C., 6 hrs), cooled to room temperature, and poured into excess 10% sodium hydroxide solution. The phases were separated and the aqueous phase was extracted twice with methylene chloride. The combined organic phase was washed three times with water and dried with anhydrous sodium sulphate. Evaporation of the solvent left a light yellow product (1.78 g) with mp. 69°-71° C., (lit. 73°-75° C., see J. Pharm. Sci. 57, 784 (1968)).

1. temperatureThe solution was heated with an oil bath (50°-70° C., 6 hrs)
2. customThe phases were separated
3. extractionthe aqueous phase was extracted twice with methylene chloride
4. washThe combined organic phase was washed three times with water
5. dry with materialdried with anhydrous sodium sulphate
6. customEvaporation of the solvent
7. waitleft a light yellow product (1.78 g) with mp. 69°-71° C., (lit. 73°-75° C., see J. Pharm. Sci. 57, 784 (1968))