HRID40578

反应详情

EQUATION

反应方程式

HRID 40578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of piperazine-1-carboxylic acid tert-butyl ester (3.5 g) and 3,4-dibromobenzaldehyde (5.0 g) in DCM (80 mL) was treated with NaB(OAc)3H (5.6 g). After 16 h, the resulting mixture was treated with 10% aq. KOH (80 mL). The aqueous phase was extracted with DCM (1×80 mL). The organic extracts were combined and dried (MgSO4). Most of the solvent was removed by concentration. Upon standing overnight, the resulting mixture produced crystals that were filtered and washed with DCM (1×5 mL), giving the title compound as a white crystalline solid (6.0 g).

WORKUP

后处理

  1. extractionThe aqueous phase was extracted with DCM (1×80 mL)
  2. dry with materialdried (MgSO4)
  3. customMost of the solvent was removed by concentration
  4. waitUpon standing overnight
  5. customthe resulting mixture produced crystals that
  6. filtrationwere filtered
  7. washwashed with DCM (1×5 mL)