反应 #792181

反应方程式

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

收率 93.0%

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

收率 93.0%

溶剂

water

ethanol

反应条件

后处理

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

实验过程

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).

来源