反应详情

130 mg (4.3 mmol) of 80% NaH are added to a solution of 0.7 g (3.5 mmol) of 4-hexylidenecyclohexanol in 20 ml of absolute THF, and the mixture is refluxed for 1 hour until deproteination is complete. 0.6 g (3.6 mmol) of 4-chloroquinazoline is subsequently added to the reaction solution at boiling point, and the mixture is refluxed for 3 hours. For working up, 2 ml of isopropanol are added. After cooling, the mixture is taken up in aqueous NH4Cl/ether and the organic phase is dried over MgSO4. Concentration of the solvent gives 1.1 g (crude product which is purified by flash chromatography (silica gel/petroleum ether:ethyl acetate=2:1)).

1. temperaturethe mixture is refluxed for 1 hour until deproteination
2. temperaturethe mixture is refluxed for 3 hours
3. temperatureAfter cooling
4. dry with materialthe organic phase is dried over MgSO4
5. customConcentration of the solvent gives
6. custom1.1 g (crude product which is purified by flash chromatography (silica gel/petroleum ether:ethyl acetate=2:1))