反应详情

To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), neopentyl glycol (208.3 g, 2.0 moles), potassium carbonate (138 g, 1.0 moles) and 500 grams methylene chloride. The batch was heated to reflux for 3 hours then cooled and clarified to remove salts. Methylene chloride was removed with a rotary evaporator and 250 grams of toluene added. The organic layer was washed with 6×50 mL of demineralized water and dried with anhydrous sodium sulfate. Toluene was removed at 3 mmHg and 75° C. to provide 244.4 g of product. GC assay of the product was 96.2%.

1. temperatureThe batch was heated
2. temperatureto reflux for 3 hours
3. temperaturethen cooled
4. customto remove salts
5. customMethylene chloride was removed with a rotary evaporator and 250 grams of toluene
6. additionadded
7. washThe organic layer was washed with 6×50 mL of demineralized water
8. dry with materialdried with anhydrous sodium sulfate
9. customToluene was removed at 3 mmHg and 75° C.