反应详情

温度

112.5 °C

In a 4-neck glass flask provided with a mechanical stirrer, condenser and thermometer 30 g of 6-iodoquinazoline-4-ol (110 mmoles), 300 mL of toluene dried on molecular sieves, 1.26 g (0.84 mL) of trifluoroacetic acid (0.1 mol. equiv.) and 79.4 g (80 mL) of 3,4-dihydro-2H-pyran (DHP) (944 mmoles; 8.6 mol. equiv.) were introduced, under nitrogen. Stirring was carried out to reflux (T=110-115° C.) for 2-3 hours and the reaction was controlled under TLC with Hexane/Ethyl Acetate (2:8) eluent. Upon completing the reaction a homogeneous solution was obtained which was cooled to ambient temperature and washed using 2×120 mL of saturated solution of sodium chloride. The organic phase was concentrated under vacuum to 40-45° C. ext T up to residue.

1. customIn a 4-neck glass flask provided with a mechanical stirrer, condenser
2. additionwere introduced, under nitrogen
3. customthe reaction a homogeneous solution
4. customwas obtained which
5. temperaturewas cooled to ambient temperature
6. washwashed
7. concentrationThe organic phase was concentrated under vacuum to 40-45° C. ext T up to residue