HRID1803490

反应详情

EQUATION

反应方程式

HRID 1803490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1,4-dichloro-6-nitro-phthalazine (1.24 g, 5.09 mmol), EtOH (20 mL), saturated aqueous NH4Cl (20 mL) and iron powder (1.42 g, 25.47 mmol) was heated to reflux for 4 h then concentrated. The residue was taken up in EtOAc washed with saturated aqueous NaHCO3, brine, dried (Na2SO4) and concentrated. Column chromatography (Hexanes/EtOAc) afforded the desired product (0.33 g, 30%) as a pale yellow solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 4 h
  3. concentrationthen concentrated
  4. washwashed with saturated aqueous NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated