HRID597395

反应详情

EQUATION

反应方程式

HRID 597395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-[(2-aminoethyl)thiomethyl]pyridine (5.0 g) and 1-nitro-2,2-bis-methylthioethylene (5.28 g) in ethanol was heated under reflux for 3 hours. Concentration and chromatographic purification of the product on a column of silica gel with elution by iso-propyl alcohol-ethylacetate (1:5) gave 1-nitro-2-methylthio-2-[2-(2-pyridylmethylthio)ethylamino]-ethylene (2.49 g), m.p. 95.5° - 96.5°.

WORKUP

后处理

  1. temperatureunder reflux for 3 hours
  2. concentrationConcentration and chromatographic purification of the product on a column of silica gel
  3. washwith elution by iso-propyl alcohol-ethylacetate (1:5)