HRID509089

反应详情

EQUATION

反应方程式

HRID 509089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of tert-butyl-4-(3-amino-4-nitrophenyl)piperazine-1-carboxylate (13 g, 46 mmol), Zn (8.9 g, 140 mmol), and HOAc (8.4 g, 140 mmol) in EtOH/THF (250 ml) was refluxed for 20 mins. After adjusted its PH to 8 by NaHCO3, EA and H2O were added resulting in a precipitate. The solid was filtered off under vacuum. The combined organic layers were dried by anhydrous Na2SO4 and concentrated in vacuo to afford tert-butyl 4-(3,4-diaminophenyl)piperazine-1-carboxylate as a black solid (8 g, yield: 60%).

WORKUP

后处理

  1. temperaturewas refluxed for 20 mins
  2. additionwere added
  3. customresulting in a precipitate
  4. filtrationThe solid was filtered off under vacuum
  5. dry with materialThe combined organic layers were dried by anhydrous Na2SO4
  6. concentrationconcentrated in vacuo