反应详情

2-Mesitylenesulfonyl chloride (5.25 g) was added to a mixture of the product from step (iii) (5 g), TEA (7 ml) and DMAP (120 mg) in DCM (100 ml) and stirred at rt for 24 h. DMF (10 ml) was added and the mixture heated under reflux for 12 h. Another portion of 2-mesitylenesulfonyl chloride (2 g) was added and heated under reflux for a further 24 h. The mixture was partitioned between DCM/water, the organics separated, washed with aq NaHCO3 soln, brine, dried and evaporated under reduced pressure. The residue was triturated with ether/isohexane and filtered to afford the subtitle compound, 9.515 g.

1. temperaturethe mixture heated
2. temperatureunder reflux for 12 h
3. temperatureheated
4. temperatureunder reflux for a further 24 h
5. customThe mixture was partitioned between DCM/water
6. washthe organics separated, washed with aq NaHCO3 soln
7. dry with materialbrine, dried
8. customevaporated under reduced pressure
9. customThe residue was triturated with ether/isohexane
10. filtrationfiltered