HRID1986164

反应详情

EQUATION

反应方程式

HRID 1986164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-(3-Bromopropyl)phthalimide (16.7 g, 62.4 mmol) is added to a stirred solution of 1-isopropyl-piperazine (8.00 g, 62.4 mmol) and diisopropylethylamine (8.06 g, 62.4 mmol) in anhydrous 1,4-dioxane (300 mL). The resultant mixture is heated in an oil bath at 90° C. for 20 hours. At ambient temperature, chloroform (300 mL) and half-saturated aqueous NaCl (200 mL) are added to the mixture. The organic layer is separated, dried over magnesium sulfate, filtered, and concentrated. The crude oil is subjected to chromatography on silica gel and eluted with 2 M NH3/CH3OH in dichloromethane 0-5% to provide the title compound as a tan oil (17.4 g, 87% yield).

WORKUP

后处理

  1. customThe organic layer is separated
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washeluted with 2 M NH3/CH3OH in dichloromethane 0-5%