HRID516532

反应详情

EQUATION

反应方程式

HRID 516532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

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 hexane-ethyl acetate).

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionthe mixture was dissolved in water (40 mL)
  3. washThe solution was washed with ethyl acetate (20 mL)
  4. extractionwas extracted with ethyl acetate (3×20 mL)
  5. customThe combined extracts were dried
  6. customevaporated
  7. customto give the product