HRID1992130
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of ethyl 3-(trifluoromethyl)-1H-pyrazole-4-carboxylate (100 mg, 0.48 mmol, 1 eq.), ethanol (5 mL) and 5N NaOH (5 mL) was heated to reflux for 72 h. The reaction was cooled to RT, acidified to pH 2 with 5 N HCl and the product extracted into ethyl acetate. The organic layers were dried over sodium sulfate, filtered and concentrated to provide 3-(trifluoromethyl) H-pyrazole-4-carboxylic acid (1a) as a white solid (80 mg, 93% yield). 1H NMR (400 MHz, DMSO-d6) δ 13.95 (broad s, 1H), 8.49 (s, 1H), 3.50 (broad s, 1H). ES-LCMS m/z 181.16 (M+H).
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 72 h
- extractionthe product extracted into ethyl acetate
- dry with materialThe organic layers were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated