反应详情

To a solution of 98.8 g of the compound obtained in Step 204-1 in DMF (455 ml) was added 72.0 g of TBSCl and 62.0 g of imidazole under ice cooling, and the reaction mixture was stirred for 10 minutes. The solution was warmed to room temperature then stirred for two hours, water and Et2O were added and liquid separation was performed. The organic layer was washed with saturated brine and dried over MgSO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. n-hexane was used on the obtained solid residue for a recovery by filtration to obtain 152 g of the title compound.

1. stirringthen stirred for two hours
2. customliquid separation
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over MgSO4
5. customthe drying agent was separated by filtration
6. customthe solvent was evaporated under reduced pressure
7. filtrationn-hexane was used on the obtained solid residue for a recovery by filtration