HRID449962

反应详情

EQUATION

反应方程式

HRID 449962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 4-oxo-1-[4-(1H-pyrazol-1-yl)benzyl]-1,4-dihydrocinnoline-3-carboxylate (750 mg, 2.00 mmol) was dissolved in toluene (9 mL), sparged under nitrogen and treated with Lawesson's Reagent (486 mg, 1.20 mmol, 0.6 equiv). The mixture was placed into an oil bath preheated to 105° C. for 1 hour, cooled to ambient temperature and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 60:40; hexanes:ethyl acetate) to provide the titled compound as a dark green solid.

WORKUP

后处理

  1. customsparged under nitrogen
  2. customThe mixture was placed into an oil bath
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by silica gel gradient chromatography (100:0 to 60:40; hexanes:ethyl acetate)