反应详情

温度

110 °C

To a solution of ethyl 5-formyl-4-methylisoxazole-3-carboxylate (Intermediate C) (50 mg, 0.273 mmol) in toluene (0.5 mL) was added 3,3-dimethylbutane-1,2-diol (32.3 mg, 0.273 mmol) and the mixture was heated at 110° C. for 4.5 hours. The resulting mixture was partitioned between EtOAc and water and the organic layer was dried over MgSO4, filtered and the solvent removed under reduced pressure. The crude material was adsorbed onto silica and purification by chromatography eluting with 0-100% EtOAc in iso-hexane afforded the title compound;

1. customThe resulting mixture was partitioned between EtOAc and water
2. dry with materialthe organic layer was dried over MgSO4
3. filtrationfiltered
4. customthe solvent removed under reduced pressure
5. customThe crude material was adsorbed onto silica and purification by chromatography
6. washeluting with 0-100% EtOAc in iso-hexane