HRID1195686

反应详情

EQUATION

反应方程式

HRID 1195686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In the manner described in Example 14, 6-methanesulfonamido-2-(4-piperidyl)-indan-1-one hydrochloride (0.20 g, 0.58 mmol), 5-(2-bromoethyl)benzofurazan (0.395 g, 1.74 mmol), sodium bicarbonate (0.146 g, 1.74 mmol) and potassium iodide (20 mg), in 20 mL of acetonitrile were heated under reflux for 30 hours. After purification by flask column chromatography on silica gel eluting with 5% methanol in chloroform saturated with ammonia (gas), and treatment with ethanol HCl, crystallization from methanol gave the title compound as a white solid, mp 214°-217° C.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureunder reflux for 30 hours
  3. customAfter purification by flask column chromatography on silica gel eluting with 5% methanol in chloroform saturated with ammonia (gas), and treatment
  4. customwith ethanol HCl, crystallization from methanol