反应详情

5-(2,4-bis-benzyloxy-5-isopropyl-phenyl)-4-(4-morpholin-4-yl-phenyl)-4H-[1,2,4]triazol-3-ol (1.2 g, 2.07 mmol) was suspended in methanol (100 mL), acetic acid (50 mL) and dimethylformamide (50 mL), and mixed with palladium carbon (60 mg), and catalytic reduction was carried out under a hydrogen atmosphere at 80° C. for 1 hour and then at room temperature overnight. After completing the reaction, the catalyst was removed by filtration and the solvent was concentrated under reduced pressure. The residue was mixed with 5% aqueous sodium hydrogencarbonate to make it neutral and then extracted twice with chloroform. The organic layer thus obtained was dried over anhydrous sodium sulfate. Sodium sulfate was removed by filtration, and the solvent was distilled off under reduced pressure, and the residue thus obtained was purified by silica gel column chromatography (dichloromethane:methanol 15:1-10:1). The obtained product was purified by suspending in ethanol to obtain the title compound (OH-a01: white crystals, 489 mg, 59%). The analytical data of this compound were the same as that of the target compound obtained in Example 2-1A.

1. customat room temperature
2. customovernight
3. customthe reaction
4. customthe catalyst was removed by filtration
5. concentrationthe solvent was concentrated under reduced pressure
6. additionThe residue was mixed with 5% aqueous sodium hydrogencarbonate
7. extractionextracted twice with chloroform
8. customThe organic layer thus obtained
9. dry with materialwas dried over anhydrous sodium sulfate
10. customSodium sulfate was removed by filtration
11. distillationthe solvent was distilled off under reduced pressure
12. customthe residue thus obtained
13. customwas purified by silica gel column chromatography (dichloromethane:methanol 15:1-10:1)
14. customThe obtained product was purified