HRID508448

反应详情

EQUATION

反应方程式

HRID 508448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 6-chlorochromone (2.00 g, 0.011 mol) in ethanol (35 mL) was added methylhydrazine sulfate (1.85 g, 0.013 mol) and triethylamine (2.0 mL, 0.014 mol) and the mixture was heated at reflux for 18 hours. After cooling to room temperature, the reaction mixture was concentrated in vacuo and the resulting residue purified by silica gel chromatography eluting with 0 to 100% EtOAc in hexane to yield two regioisomeric products in a 1:4 ratio, the title compound being the minor regiosiomer.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 18 hours
  3. concentrationthe reaction mixture was concentrated in vacuo
  4. customthe resulting residue purified by silica gel chromatography
  5. washeluting with 0 to 100% EtOAc in hexane
  6. customto yield two regioisomeric products in a 1:4 ratio