반응 #792181

반응 방정식

Potassium hydroxide

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

product

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

→

product

수율 93.0%

1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid

수율 93.0%

용매

water

ethanol

반응 조건

후처리

1. 1
   기타the solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONthe mixture was dissolved in water (40 mL)
3. 3
   세척The solution was washed with ethyl acetate (20 mL)
4. 4
   추출was extracted with ethyl acetate (3×20 mL)
5. 5
   기타The combined extracts were dried
6. 6
   기타evaporated
7. 7
   기타to give

실험 절차

Potassium hydroxide (0.5 g, 85%, 2.28 mmol) in water (1 mL) was added to ethyl 1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxylate (i.e. the product of Step D) (0.66 g, 2.07 mmol) in ethanol (3 mL). After about 30 minutes, the solvent was removed under reduced pressure, and the mixture was dissolved in water (40 mL). The solution was washed with ethyl acetate (20 mL). The aqueous layer was acidified with concentrated hydrochloric acid and was extracted with ethyl acetate (3×20 mL). The combined extracts were dried and evaporated to give the product as a solid (0.53 g, 93% yield), m.p. 178-179° C. (after crystallization from hexanes-ethyl acetate).

출처