431-03-8

149-73-5

21983-72-2

The general procedure for the synthesis of 3,3-dimethoxy-2-butanone from 2,3-butanedione and trimethyl orthoformate was as follows: 2,3-butanedione (47.3 g, 0.55 mol) was added to a reaction flask equipped with a stirrer, and a mixture of trimethyl orthoformate (64.13 g, 0.605 mol) and p-toluenesulfonic acid (0.19 g) was slowly added dropwise at 15 °C. The reaction temperature was maintained at 15 °C and the reaction was continuously stirred for 7 h to ensure complete reaction. After completion of the reaction, potassium carbonate (1 g) was added to neutralize the reaction mixture and stirring was continued for 1 hour. Subsequently, distillation was carried out under reduced pressure at 100 mmHg and the crude product was collected. For further purification, the crude product was subjected to secondary distillation at 90 °C and 200 mbar. The yield of the final product was 83%.