反应详情

At 0 to 5° C., the 2,4-dichloro-3-(3-methylisoxazol-5-yl)benzoyl chloride obtained above (step e) in 40 ml of dimethoxyethane was added to 0.7 g (7.35 mmol) of 5-hydroxy-1-methyl-1H-pyrazole in 30 ml of dimethoxyethane and 2.0 g (14.7 mmol) of potassium carbonate. The mixture was stirred at room temperature for 3.5 hours, heated under reflux for 1 hour and stirred at room temperature for 12 hours. The precipitate that had formed was filtered off with suction and introduced into 50 ml of water. The mixture is acidified to pH=1 and the solid is filtered off with suction and dried. Likewise, the first-mentioned filtrate was taken up in 400 ml of water, washed with methyl t-butyl ether, adjusted to pH 3 and extracted with methylene chloride. The combined organic phases were dried and concentrated. 1.9 g (73% of theory) of 4-[2,4-dichloro-3-(3-methylisoxazol-5-yl)benzoyl]-5-hydroxy-1-methyl-1H-pyrazole were obtained.

1. temperatureheated
2. temperatureunder reflux for 1 hour
3. stirringstirred at room temperature for 12 hours
4. customThe precipitate that had formed
5. filtrationwas filtered off with suction
6. additionintroduced into 50 ml of water
7. filtrationthe solid is filtered off with suction
8. customdried
9. washwashed with methyl t-butyl ether
10. extractionextracted with methylene chloride
11. customThe combined organic phases were dried
12. concentrationconcentrated