تفاعل #792180

معادلة التفاعل

ethyl 1-(3-chloro-2-pyridinyl)-4,5-dihydro-5-hydroxy-3-(trifluoromethyl)-1H-pyrazole-5-carboxylate

product

ethyl 1-(3-chloro-2-pyridinyl)-4,5-dihydro-5-hydroxy-3-(trifluoromethyl)-1H-pyrazole-5-carboxylate

→

product

المردود 77.0%

ethyl 1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxylate

المردود 77.0%

المذيبات

acetic acid

acetic acid

ظروف التفاعل

المعالجة

1. 1
   أخرىwas removed under reduced pressure
2. 2
   أخرىThe mixture was partitioned between saturated aqueous sodium carbonate solution (100 mL) and ethyl acetate (100 mL)
3. 3
   استخلاصThe aqueous layer was further extracted with ethyl acetate (100 mL)
4. 4
   أخرىThe combined organic extracts were dried
5. 5
   أخرىevaporated

الإجراء التجريبي

Sulfuric acid (concentrated, 2 drops) was added to ethyl 1-(3-chloro-2-pyridinyl)-4,5-dihydro-5-hydroxy-3-(trifluoromethyl)-1H-pyrazole-5-carboxylate (i.e. the product of Step C) (1 g, 2.96 mmol) in acetic acid (10 mL) and the mixture was warmed to 65° C. for about 1 hour. The mixture was allowed to cool to 25° C. and most of the acetic acid was removed under reduced pressure. The mixture was partitioned between saturated aqueous sodium carbonate solution (100 mL) and ethyl acetate (100 mL). The aqueous layer was further extracted with ethyl acetate (100 mL). The combined organic extracts were dried and evaporated to give the product as an oil (0.66 g, 77% yield).

المصدر