反应详情

温度

65 °C

5-(4-(1H-1,2,4-triazol-1-yl)benzyl)-2,2-dimethyl-1,3-dioxane-4,6-dione (10.0 g, 33.2 mmol, Intermediate 45, step b) was dissolved in a mixture of water (30 mL) and trifluoroacetic acid (50 mL). The mixture was heated to 65° C. After 2.5 hours, the mixture was allowed to cool to 23° C. Water and trifluoroacetic acid were removed by rotary evaporation at 45° C. Toluene (100 mL) was added to the residue then the mixture was concentrated by rotary evaporation at 45° C. Tetrahydrofuran (100 mL) and 6 M aqueous hydrochloric acid solution (28 mL) was added to the residue in sequence. The resulting heterogeneous mixture was stirred at 23° C. After 10 minutes, the mixture was concentrated by rotary evaporation at 45° C. Tetrahydrofuran (100 mL) was added to the residue and the mixture concentrated by rotary evaporation at 45° C. Toluene (100 mL) was added to the residue and the mixture concentrated by rotary evaporation at 45° C. The resulting white solid was dried under vacuum at 40° C. The solid product was used directly in the next step without further purification.

1. temperatureto cool to 23° C
2. customWater and trifluoroacetic acid were removed by rotary evaporation at 45° C
3. additionToluene (100 mL) was added to the residue
4. concentrationthe mixture was concentrated by rotary evaporation at 45° C
5. additionTetrahydrofuran (100 mL) and 6 M aqueous hydrochloric acid solution (28 mL) was added to the residue in sequence
6. waitAfter 10 minutes
7. concentrationthe mixture was concentrated by rotary evaporation at 45° C
8. additionTetrahydrofuran (100 mL) was added to the residue
9. concentrationthe mixture concentrated by rotary evaporation at 45° C
10. additionToluene (100 mL) was added to the residue
11. concentrationthe mixture concentrated by rotary evaporation at 45° C
12. customThe resulting white solid was dried under vacuum at 40° C
13. customThe solid product was used directly in the next step without further purification