反应详情

A solution of the product from Step 1 (92 g, 0.28 mol) in DCM (1200 mL) was cooled to 0° C., and HCl was bubbled through the solution for 10 minutes. The cooling bath was then removed, and the reaction mixture stirred for 2 hours. N2 was bubbled through the reaction mixture for 5 minutes, and the volatiles evaporated. The residue was azeotroped with DCM (3×) to give an off-white powder (75 g). LRMS (M+H)+ Calcd.=233. found 233.

1. customHCl was bubbled through the solution for 10 minutes
2. customThe cooling bath was then removed
3. customN2 was bubbled through the reaction mixture for 5 minutes
4. customthe volatiles evaporated
5. customThe residue was azeotroped with DCM (3×)