HRID82202
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of (1-Cyclopropyl-5-trifluoromethyl-1H-pyrazol-4-yl)-acetonitrile (Preparation 139, 700 mg, 3.25 mmol) in EtOH (15 mL) was added aqueous 1N NaOH (15 mL). The resulting solution was heated at 60° C. for 16 hours. The mixture was concentrated and the residue was dissolved in water (10 mL) and washed with EtOAc. The pH of aqueous layer was adjusted to 5 using 1N HCl and extracted with 10% IPA in DCM (4×30 mL). The organic layer was dried (Na2SO4) and evaporated in vacuo to afford the title compound as a solid in 85% yield, 650 mg.
WORKUP
后处理
- concentrationThe mixture was concentrated
- dissolutionthe residue was dissolved in water (10 mL)
- washwashed with EtOAc
- extractionextracted with 10% IPA in DCM (4×30 mL)
- dry with materialThe organic layer was dried (Na2SO4)
- customevaporated in vacuo