反応 #792181

反応方程式

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

収率 93.0%

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

収率 93.0%

溶媒

water

ethanol

反応条件

後処理

1. 1
   その他the solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONthe mixture was dissolved in water (40 mL)
3. 3
   洗浄The solution was washed with ethyl acetate (20 mL)
4. 4
   抽出was extracted with ethyl acetate (3×20 mL)
5. 5
   その他The combined extracts were dried
6. 6
   その他evaporated
7. 7
   その他to give

実験手順

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).

出典