HRID1852409

反应详情

EQUATION

反应方程式

HRID 1852409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pyrrolidine (1.5 mL, 18.3 mmol) was added to a stirred solution of 3-nitrophenyl isocyanate (1.5 g, 9.14 mmol) in anhydrous THF (60 mL) and the mixture stirred at reflux for 1 hour. The solvent was evaporated in vacuo. The crude product was then purified by column chromatography (Flashmaster, 40-63 mesh silica gel, 50% isohexane-EtOAc) to provide the title compound as an off white solid (1.85 g, 86%); LC-MS, Rt=2.80 min (MeOH-FA), m/z 236 (MH+).

WORKUP

后处理

  1. temperatureat reflux for 1 hour
  2. customThe solvent was evaporated in vacuo
  3. customThe crude product was then purified by column chromatography (Flashmaster, 40-63 mesh silica gel, 50% isohexane-EtOAc)