反应详情

温度

100 °C

A 1 liter reactor equipped with a reflux condenser and magnetic stirring bar was charged under argon with 45 g of 4-chloroacetyl-catechol of a purity of ca. 90%, 260 ml of ethanol, 130 ml of water, 38 g of sodium formate and 17 ml (˜21 g) of formic acid. The stirred mixture was heated under reflux (˜100° C.) for 24 hours. Under vacuum a part of the solvents was distilled off. The remaining solution of about 100 ml was acidified by addition of 35.5 g of conc. hydrochloric acid (37%) resulting in a pH of about 0.5. 200 ml of water were added and the mixture was refluxed for 10 minutes. Upon stirring over night without heating crystals separated. The slurry was filtered by suction and the crystals were washed with 50 ml of cold water. After drying over night at 70° C. at ˜20 mbar the yield of 4-hydroxyacetyl-catechol was 34.2 g with a purity of 89.2% corresponding to a yield of 82.6%. In the mother liquors additional 14% of the product was detected by analysis.

1. customA 1 liter reactor equipped with a reflux condenser and magnetic stirring bar
2. temperatureThe stirred mixture was heated
3. distillationUnder vacuum a part of the solvents was distilled off
4. additionThe remaining solution of about 100 ml was acidified by addition of 35.5 g of conc. hydrochloric acid (37%)
5. customresulting in a pH of about 0.5
6. temperaturethe mixture was refluxed for 10 minutes
7. temperaturewithout heating crystals
8. customseparated
9. filtrationThe slurry was filtered by suction
10. washthe crystals were washed with 50 ml of cold water
11. dry with materialAfter drying over night at 70° C. at ˜20 mbar the yield of 4-hydroxyacetyl-catechol