反应详情

温度

110 °C

To a stirred mixture of 1-Methyl-5-phenoxy-1H-pyrazole-4-carboxylic acid (16.00 g; 73.32 mmol), t-BuOH (51.20 g; 690.77 mmol) in 1,4-dioxane under argon was added DIPEA (37.44 g; 289.69 mmol) and Diphenylphosphoryl azide (41.60 g; 151.16 mmol). After 10 minutes at ambient temperature it was heated up to 110° C. and stirred there for 3 hours. The solvent was evaporated and the crude material purified by column chromatography. This compound was dissolved in DCM and treated with 4 M HCl in 1,4-dioxane. It was stirred for 2 days at ambient temperature. The solvent was evaporated and the residue dissolved in water and washed with EtOAc. The aqueous layer was basified with NaHCO3 solution and extracted with EtOAc. The organic layer was dried and concentrated to dryness.

1. customThe solvent was evaporated
2. customthe crude material purified by column chromatography
3. dissolutionThis compound was dissolved in DCM
4. additiontreated with 4 M HCl in 1,4-dioxane
5. stirringIt was stirred for 2 days at ambient temperature
6. customThe solvent was evaporated
7. dissolutionthe residue dissolved in water
8. washwashed with EtOAc
9. extractionextracted with EtOAc
10. customThe organic layer was dried
11. concentrationconcentrated to dryness