反应详情

To a solution of 99.7 g (0.513 mole) of 2,4-dihydroxy-3-propylacetophenone and 72.7 g (0.77 mole) of dimethyl oxalate in 1 liter of dry dimethylformamide was added in portions 97 g (1.8 mmole) of sodium methoxide. After stirring for 4 hours, 1.8 l of acetic acid was added and stirring was continued for 4 days. The reaction mixture was heated in a steam bath for four hours and evaporated to dryness. Water was added to the residue and the mixture was heated to boiling. A solid was filtered off and recrystallized from ethanol to give 89.8 g of the title compound, mp. 222°-224°. Structure assignment was supported by nmr and infrared spectra.

1. stirringstirring
2. waitwas continued for 4 days
3. temperatureThe reaction mixture was heated in a steam bath for four hours
4. customevaporated to dryness
5. additionWater was added to the residue
6. temperaturethe mixture was heated to boiling
7. filtrationA solid was filtered off
8. customrecrystallized from ethanol