反应详情

0.42 g (17.5 mmol) of NaH (80% pure) was added in portions to a solution of 1.8 g (12.8 mmol) of cis-4isopropenylcyclohexanol in 20 ml of absolute THF. The mixture was then heated at reflux for 3 hours, and a solution of 1.9 g (11.6 mmol) of 4-chloroquinazoline in 10 ml of THF was added dropwise. The reaction mixture was subsequently heated at reflux for 5 hours. After cooling to room temperature, 10 ml of isopropanol were added, the mixture was subsequently stirred for 15 minutes, and the reaction solution was poured into saturated ammonium chloride solution. Extraction was carried out with ether, the combined organic phases were dried over MgSO4 and the solvent was concentrated by evaporation in vacuo. The residue (2.7 g) was purified by flash chromatography over silica gel with petroleum ether/ethyl acetate 3:1. After concentration, 1.8 g (57.6% of theory) were obtained of a colorless oil.

1. temperatureThe mixture was then heated
2. temperatureat reflux for 3 hours
3. temperatureThe reaction mixture was subsequently heated
4. temperatureat reflux for 5 hours
5. extractionExtraction
6. dry with materialthe combined organic phases were dried over MgSO4
7. concentrationthe solvent was concentrated by evaporation in vacuo
8. customThe residue (2.7 g) was purified by flash chromatography over silica gel with petroleum ether/ethyl acetate 3:1
9. concentrationAfter concentration
10. custom1.8 g (57.6% of theory) were obtained of a colorless oil