HRID2377699

反应详情

EQUATION

反应方程式

HRID 2377699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Amino-2-pyridinethiol (5.0 g, 39.6 mmol) and 2-chloro-1,1,1-triethoxyethane (8.57 g, 43.5 mmol) were combined in absolute ethanol (40 mL) and refluxed for 2 hours. The mixture was concentrated under reduced pressure and the residue purified by flash chromatography (ethyl acetate:hexanes, 1:4) to provide the title compound. 1H NMR (300 MHz, CDCl3) δ 4.93 (s, 2H) 7.47 (dd, J=8.14, 4.75 Hz, 1H) 8.26 (dd, J=8.31, 1.53 Hz, 1H) 8.62 (dd, J=4.58, 1.53 Hz, 1H). (ESI) m/z 186 (M+H)+.

WORKUP

后处理

  1. temperaturerefluxed for 2 hours
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue purified by flash chromatography (ethyl acetate:hexanes, 1:4)