HRID748330

反应详情

EQUATION

反应方程式

HRID 748330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Cyanopyridine (0.29 g, 2.8 mmol) and 4-bromothiosalicylic acid (0.8 g, 3.4 mmol) were dissolved in pyridine (6 ml), and the mixture was refluxed for 8 hrs. The solvent was evaporated, and the residue was subjected to silica gel column chromatography. The fractions eluted with chloroform-ethyl acetate (5:1, v/v) were collected, concentrated and recrystallized from hexane-chloroform to give the titled compound (0.33 g, 36%) as white crystals.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 8 hrs
  2. customThe solvent was evaporated
  3. washThe fractions eluted with chloroform-ethyl acetate (5:1
  4. customv/v) were collected
  5. concentrationconcentrated
  6. customrecrystallized from hexane-chloroform