反应详情

温度

60 °C

A solution of (R)-2-(3,4-dichlorobenzenesulfonamido)-N-(2,2-dimethoxyethyl)pent-4-ynamide (36.7 g, 89.6 mmol) in 500 mL p-dioxane was treated with TsOH.H2O (5.11 g, 26.9 mmol). The reaction was heated to 60° C. for 7 h and then at 80° C. for 19 h. The mixture was cooled to room temperature and concentrated under reduced pressure. The residue was diluted with 400 mL EtOAc stirred with 400 mL 5% NaHCO3. The resulting precipitate was filtered and washed with H2O. The solid was suspended in hot EtOH and cooled to rt. The solid was collected by filtration, washed with EtOH and dried in vacuo to yield the title compound.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. additionThe residue was diluted with 400 mL EtOAc
4. filtrationThe resulting precipitate was filtered
5. washwashed with H2O
6. temperaturecooled to rt
7. filtrationThe solid was collected by filtration
8. washwashed with EtOH
9. customdried in vacuo