反应详情

温度

62.5 °C

The wet product obtained in Example 1 (Voriconazole (1R)-(−)-10-camphorsulfonate, 41.49 g wet, 40.36 g dry estimated, 0.069 mol) was suspended in ethyl acetate (121 ml) and aqueous saturated sodium bicarbonate solution (97 ml) was added slowly. The mixture was stirred for 10 minutes, the phases allowed to settle and the organic layer separated. The aqueous layer was re-extracted with ethyl acetate (91 ml). The combined organic layers were washed with deionised water (12 ml), filtered and concentrated under vacuum until a white doughy residue was obtained. Isopropanol (24 ml) was added and concentrated again under vacuum until a white doughy residue was obtained. Isopropanol (54.5 ml) was added and the suspension was heated until complete solution (60-65° C.). The solution was cooled down to 0-2° C. and stirred for at least 1 hour. The suspension formed was filtered, the cake was washed with cold isopropanol (6.1 ml). A white crystalline solid was obtained after drying at 55-60° C. under vacuum until constant weight: 19.75 g (81.43% yield).

1. customthe organic layer separated
2. extractionThe aqueous layer was re-extracted with ethyl acetate (91 ml)
3. washThe combined organic layers were washed with deionised water (12 ml)
4. filtrationfiltered
5. concentrationconcentrated under vacuum until a white doughy residue
6. customwas obtained
7. concentrationconcentrated again under vacuum until a white doughy residue
8. customwas obtained
9. temperatureThe solution was cooled down to 0-2° C.
10. stirringstirred for at least 1 hour
11. customThe suspension formed
12. filtrationwas filtered
13. washthe cake was washed with cold isopropanol (6.1 ml)
14. customA white crystalline solid was obtained
15. customafter drying at 55-60° C. under vacuum until constant weight