HRID1090047

反应详情

EQUATION

反应方程式

HRID 1090047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1,2-Bis (2-mercapto-2-methylpropylamino)benzene (0.17 g, 6.1×10-4 mol, 120 M%) and 0.07 g (5.1×10-4 mol, 100 M%) 1- bromobutane were dissolved in 25 ml tetrahydrofuran (freshly distilled over Na). Sodium hydride (0.03 g, 6.25×10-4 mol, 102 M%) was then added. The mixture was stirred at room temperature under nitrogen for 3 hours. The reaction mixture was worked up as in Example 40. The product was isolated by radial chromatography on 1 mm silica plate, using hexane: ethyl acetate as the eluting solvent, giving 40 mg (23% yield) 2-(2-butylthio-2-methylpropylamino]-1-(2-mercapto-2-methylpropylamino)benzene as a yellow oil.

WORKUP

后处理

  1. distillationfreshly distilled over Na)
  2. customThe product was isolated by radial chromatography on 1 mm silica plate