反应详情

温度

100 °C

A 0.1 liter reactor equipped with a reflux condenser and magnetic stirring bar was charged under argon with 5.05 g of 4-chloroacetyl-catechol of a purity of ca. 99%, 50 ml of water, 2.8 g of sodium formate and 1.55 ml (˜1.9 g) of formic acid. The stirred mixture was heated under reflux (˜100° C.) for 22 hours. The solution was cooled to about 25° C. and acidified by addition of 2 g of conc. hydrochloric acid (37%) resulting in a pH of about 0.5. The mixture was extracted with ethyl acetate, once with 100 ml then 3 times with 50 ml each. The organic extracts have been back washed 3 times with 30 ml 10% brine. The combined organic phases were dried with sodium sulfate, filtered and evaporated at reduced pressure at 40° C. This resulted in a light tan solid crystalline product of 4.56 g of 97.4% purity corresponding to a yield of 98.9%.

1. customA 0.1 liter reactor equipped with a reflux condenser and magnetic stirring bar
2. temperatureThe stirred mixture was heated
3. temperatureThe solution was cooled to about 25° C.
4. customresulting in a pH of about 0.5
5. extractionThe mixture was extracted with ethyl acetate, once with 100 ml
6. washThe organic extracts have been back washed 3 times with 30 ml 10% brine
7. dry with materialThe combined organic phases were dried with sodium sulfate
8. filtrationfiltered
9. customevaporated at reduced pressure at 40° C
10. customThis resulted in a light tan solid crystalline product of 4.56 g of 97.4% purity corresponding to a yield of 98.9%