反应详情

Dissolved in 500 ml of dichloromethane were 29 g (165.7 mmol) of 3-phenyl-5-hydroxymethylisoxazole prepared in Example 28 and 80 g of "Florisil" (trade mark), followed by the addition of 74 g (342.6 mmol) of pyridinium chlorochromate. They were reacted for 7 hours at room temperature. After an insoluble material was filtered off, the filtrate was added into water and then extracted with dichloromethane. After the solvent was distilled off, the residue was purified by silica gel chromatography (eluent: chloroform) so that 3-phenylisoxazole-5-aldehyde was obtained as crystals. Analytical results of the crystals obtained: Yield: 26.0 g (90.7%). Melting point: 67°-69° C.

1. customThey were reacted for 7 hours at room temperature
2. filtrationAfter an insoluble material was filtered off
3. additionthe filtrate was added into water
4. extractionextracted with dichloromethane
5. distillationAfter the solvent was distilled off
6. customthe residue was purified by silica gel chromatography (eluent: chloroform) so that 3-phenylisoxazole-5-aldehyde
7. customwas obtained as crystals
8. customAnalytical results of the crystals
9. customobtained