反应详情

温度

115 °C

A solution of ethyl 6-amino-3-methoxy-4-(1-methylpiperidin-4-ylmethoxy)benzoate (16.1 g, 50 mmol) in 2-methoxyethanol (160 ml) containing formamidine acetate (5.2 g, 50 mmol) was heated at 115° C. for 2 hours. Formamidine acetate (10.4 g, 100 mmol) was added in portions every 30 minutes over a period of 4 hours and the reaction was heated for 30 minutes after the last addition. The reaction was cooled, the volatiles were removed in vacuo, and the residue was dissolved in ethanol (100 ml) and dichloromethane (50 ml). The reaction was filtered and the filtrate was concentrated to a final volume of 100 ml. Collection of the precipitated solid by suction filtration (at 5° C.) followed by drying in vacuo yielded 6-methoxy-7-((1-methylpiperidin-4-yl)methoxy)-3,4-dihydroquinazolin-4-one (12.7 g, 70% yield) as a white solid:

1. temperaturethe reaction was heated for 30 minutes
2. additionafter the last addition
3. temperatureThe reaction was cooled
4. customthe volatiles were removed in vacuo
5. dissolutionthe residue was dissolved in ethanol (100 ml)
6. filtrationThe reaction was filtered
7. concentrationthe filtrate was concentrated to a final volume of 100 ml
8. customCollection of the precipitated solid
9. filtrationby suction filtration (at 5° C.)
10. customby drying in vacuo