反应详情

温度

30 °C

A suspension of the product from step (ii) (6.0 g, 23.6 mmol), 2,4,6-triisopropylbenzenesulfonyl chloride (9.28 g, 30.6 mmol) and DABCO (4.76 g, 42.5 mmol) in THF (48.0 g) was stirred at 30° C. for 7 hours. Water (9.6 g) was added to the mixture and the organic layer was separated and concentrated under reduced pressure to give a solid. The solid was dissolved in acetonitrile (57.0 g) and heated to 60° C. Water (36.0 g) was added to the solution and the mixture was stirred at 60° C. for 1 hour. Water (36.0 g) was added to the mixture and the mixture was cooled to 5° C. and stirred at 5° C. for 1 hour. The resulting precipitate was collected by filtration, washed duplicate with combined solution of water (9.0 g) and acetonitrile (3.6 g), and dried to give the subtitle is compound as a solid, 11.6 g.

1. customthe organic layer was separated
2. concentrationconcentrated under reduced pressure
3. customto give a solid
4. temperatureheated to 60° C
5. stirringthe mixture was stirred at 60° C. for 1 hour
6. temperaturethe mixture was cooled to 5° C.
7. stirringstirred at 5° C. for 1 hour
8. filtrationThe resulting precipitate was collected by filtration
9. washwashed duplicate with combined solution of water (9.0 g) and acetonitrile (3.6 g)
10. customdried
11. customto give the subtitle