1, 4-disubstituted 3, 4-dihydro-2 (3H)-quinazolinone compound as well as synthesis method and application thereof
A technology of quinazolinones and compounds, applied in the field of organic synthesis and medicine, capable of solving problems that have not yet been reported
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Embodiment 1
[0087] Example 1 Compound 2a
[0088]
[0089] Under nitrogen protection, magnesium (0.4g, 17.8mmol) was added to tetrahydrofuran THF (20mL), then a grain of iodine (diameter 0.2mm, about 10mg) was added, and heated to 70°C. Then 2-methylbromobenzene (3 g, 17.5 mmol) was added and reacted at 70° C. for 1 hour. Afterwards, the solution was transferred to a THF solution (20 mL) of 2-nitrobenzaldehyde (2.65 g, 17.5 mmol) and reacted at room temperature for 1 hour. After the reaction solution was quenched with water, it was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, and dried over anhydrous sodium sulfate. Solvent was removed using a rotary evaporator. The obtained crude product was purified by silica gel column chromatography. The product 3.6g (14.8mmol) was obtained, the yield was 85%, white solid.
Embodiment 2
[0090] Example 2 compound 3a example
[0091] Compound 3a
[0092]
[0093] Chromium trioxide pyridine hydrochloride (PCC) (90mmol) in dichloromethane (20mL) was added dropwise to compound 2a (3.6g, 14.8mmol) in dichloromethane (50mL) at room temperature, stirred at room temperature for 5h , the reaction solution was filtered through celite, washed with ether, and the solvent was removed by a rotary evaporator. The obtained crude product was purified by silica gel column chromatography to obtain 3.2 g (13.2 mmol) of the product, with a yield of 90%, as a pale yellow solid.
Embodiment 3
[0094] Example 3 Compound 4 Example
[0095] Compound 4a
[0096]
[0097] Compound 3a (3g, 12.4mmol), ethanol (15mL), water (15mL) and iron powder (14g, 249mmol) were mixed and heated at 40°C for 30 minutes, then hydrochloric acid (2mL, 12mol / L) was added, and React for 2 hours. The solution was filtered through celite and washed with saturated sodium bicarbonate. After extraction with dichloromethane, the organic layer was dried over anhydrous sodium sulfate. Solvent was removed by rotary evaporator. The obtained crude product was purified by silica gel column chromatography. The product was obtained in 2.5 g (12 mmol), 95% yield, as a pale yellow solid.
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