HRID1647807

反应详情

EQUATION

反应方程式

HRID 1647807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 4-(3-methoxy-4-pyridinyl)-1-piperazinecarboxylate (1.2 g, 4.7 mmol) in 50 mL of EtOH containing 1 mL of 85% hydrazine hydrate and potassium hydroxide (12 g, 210 mol) was heated to reflux for 12 h. The reaction mixture was cooled, concentrated in vacuo and the residue dissolved in EtOAc. The organic extracts were dried (brine, MgSO4), filtered and concentrated in vacuo. Silica gel chromatography (3:1:0.01 CH2Cl2 -MeOH-Et3N) of the residue gave the desired compound (0.42 g, 46%).

WORKUP

后处理

  1. temperatureto reflux for 12 h
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated in vacuo
  4. dissolutionthe residue dissolved in EtOAc
  5. dry with materialThe organic extracts were dried (brine, MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo