反应详情

温度

110 °C

A mixture of crude Intermediate 3-(dimethylamino)-1-(3-iodo-1-isopropyl-1H-pyrazol-4-yl)prop-2-en-1-one (4.0 g, 12.0 mmol), guanidine hydrochloride (2.63 g, 27.6 mmol), lithium hydroxide (635 mg, 27.6 mmol), and sec-butanol (50 ml) was heated with stirring in a sealed reaction vessel at 110° C. for 20 h. The cooled reaction mixture was concentrated, then water was added and the mixture was extracted with ethyl acetate. The combined extracts were dried over sodium sulfate, filtered, and concentrated. Ethyl acetate was added to the solid residue, and the mixture was sonicated. The solid product was collected on a filter, rinsed with ethyl acetate, and dried to give the title compound as a tan solid. MS m/z 330.0 (M+1).

1. temperaturewas heated
2. customThe cooled reaction mixture
3. concentrationwas concentrated
4. additionwater was added
5. extractionthe mixture was extracted with ethyl acetate
6. dry with materialThe combined extracts were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. additionEthyl acetate was added to the solid residue
10. customthe mixture was sonicated
11. customThe solid product was collected on a filter
12. washrinsed with ethyl acetate
13. customdried