HRID2045690

反应详情

EQUATION

反应方程式

HRID 2045690 反应方程式

PROCEDURE

实验过程

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 was bubbled through the solution. After 10 min, the cooling bath was removed, and the reaction mixture was 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.

WORKUP

后处理

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