反应详情

温度

65 °C

2. Approximately 509 g of the starting compound, salicylaldehyde (1) was introduced into a 4-liter Erlenmeyer flask with powdered potassium carbonate (569 g), dimethylformamide (1,000 ml), and methyl chloroacetate (478 g) and mechanically stirred at 65° C. for about 24 hours. The stirring was stopped and the reaction mixture cooled to 25° C. The mixture was poured into cold water (0° C.) while stirring vigorously. An oil separated that suddenly solidified. Stirring was continued for 30 minutes and the solid isolated by filtration. The product was washed with water (2×1,000 ml) and pressed dry. The product can also be dried in vacuo at 25° C. A small sample (approx. 2 g) was purified by distillation. The boiling range of the pure product is 124°-128° C. at 2 mm Hg and has a melting temperature range of about 50.2°-50.6° C.

1. temperaturethe reaction mixture cooled to 25° C
2. stirringwhile stirring vigorously
3. customAn oil separated
4. stirringStirring
5. waitwas continued for 30 minutes
6. customthe solid isolated by filtration
7. washThe product was washed with water (2×1,000 ml)
8. custompressed dry
9. customThe product can also be dried in vacuo at 25° C
10. distillationA small sample (approx. 2 g) was purified by distillation
11. customis 124°-128° C. at 2 mm Hg
12. customa melting temperature range of about 50.2°-50.6° C.