反应详情

温度

100 °C

A 2M solution of HCl in H2O was added to a solution of 5-phenoxymethyl-2H-pyrazole-3-carboxylic acid (2,2-dimethoxy-ethyl)-amide (1.25 g, 4.09 mmol) in acetone (7 mL). The mixture was stirred at 100° C. for 5 minutes under microwave irradiation. The solvent was evaporated in vacuo and the residue was supported on silica gel and purified by flash column chromatography (silica; AcOEt in DCM 0/100 to 100/0, then MeOH in AcOEt 0/100 to 10/90). Desired fractions were collected and the solvents evaporated in vacuo. The residue was triturated with diethyl ether to yield (rac)-7-hydroxy-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (286 mg, 30% yield) as an off-white solid.

1. customThe solvent was evaporated in vacuo
2. custompurified by flash column chromatography (silica
3. customDesired fractions were collected
4. customthe solvents evaporated in vacuo
5. customThe residue was triturated with diethyl ether