反应详情

A solution of the product from Step 1 above (92 g, 0.28 mol) in DCM (1200 mL) was cooled to 0° C. and HCl bubbled through the solution for 10 min, the cooling bath removed and the reaction mixture stirred for 2 h. Nitrogen was bubbled through the reaction mixture for 5 min 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 bubbled through the solution for 10 min
2. customthe cooling bath removed
3. customNitrogen was bubbled through the reaction mixture for 5 min
4. customthe volatiles evaporated
5. customThe residue was azeotroped with DCM (×3)