HRID1493186

反应详情

EQUATION

反应方程式

HRID 1493186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Methanesulphonylcarbonimidodithioic acid dimethyl ester (3 g) and 3-[3-aminopropoxy]-N,N-dimethylbenzenemethanamine (2.5 g) were heated at reflux in ethanol for 4 hours. Methylamine was then added and the reflux continued for 11/2 hours. The solvent was removed and the residue was purified by column chromatography on silica with methanol to yield the title compound as a yellow gum (1.9 g). TLC methanol:0.88 ammonia (80:1) Rf 0.65. NMR (CDCl3) 2.85 m (1H); 2.9-3.3 m (3H); 3.0-4.3 brs (2H); 5.90 t (2H); 6.5 q (2H); 6.6 s (2H); 7.1 s (6H); 7.75 s (6H); 7.9 m (2H).

WORKUP

后处理

  1. custom2 hours
  2. customThe solvent was removed
  3. customthe residue was purified by column chromatography on silica with methanol