반응 #8155

반응 방정식

phenyl hydrazine

2-acetyl-3-oxo-butyric acid ethyl ester

pyridine

→

product

3,5-dimethyl-1-phenyl-1H-pyrazole-4-carboxylic acid ethyl ester

용매

ethanol

반응 조건

후처리

1. 1
   기타The solvents were removed under vacuum
2. 2
   세척The resulting suspension was washed with 5% sodium bicarbonate, 5% hydrochloric acid
3. 3
   건조The organic layer was dried over NaSO4
4. 4
   여과the solids filtered
5. 5
   기타the solvents removed under vacuum
6. 6
   기타The crude material was purified over silica gel

실험 절차

Similar to Example 1, phenyl hydrazine (7.5 mmol, 0.8 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (7.5 mmol, 1.3 g) were mixed in a solution of 50% pyridine in ethanol. The solvents were removed under vacuum and the oil resuspended in chloroform. The resulting suspension was washed with 5% sodium bicarbonate, 5% hydrochloric acid, and then brine. The organic layer was dried over NaSO4, the solids filtered, and the solvents removed under vacuum. The crude material was purified over silica gel to yield the named product as an oil. 1H-NMR (CDCl3, ppm): 1.37 t (3H); 2.51 s (6H); 4.32 q (2H); 7.42 bs (5H).

출처