反应详情

温度

60 °C

According to Scheme 1 Step 2: A solution of LiOH (358 mmol, 15.3 g) in water (2 M) was added at room temperature to a solution of ethyl 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxylate (143 mmol, 37.2 g) in THF/MeOH (1:1, 400 mL) and the reaction mixture was heated at 60° C. overnight. After evaporation of THF and MeOH, a solid was filtered, water (150 mL) was added and the aqueous phase was extracted with Et2O. The aqueous phase was then acidified with a solution of HCl 1 M until pH=1-2 and extracted with DCM. The organic phase was washed with brine, was dried over MgSO4, was filtered and was concentrated under reduced pressure to yield 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxylic acid (138 mmol, 32.1 g, 97%) as a pale yellow solid. The crude product was used without further purification.

1. customAfter evaporation of THF and MeOH
2. filtrationa solid was filtered
3. additionwater (150 mL) was added
4. extractionthe aqueous phase was extracted with Et2O
5. extractionextracted with DCM
6. washThe organic phase was washed with brine
7. dry with materialwas dried over MgSO4
8. filtrationwas filtered
9. concentrationwas concentrated under reduced pressure