HRID1966057

反应详情

EQUATION

反应方程式

HRID 1966057 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-amino-5-(trifluoromethoxy)phenylthio]-acetonitrile (0.70 g, 2.82 mmol) in 5% EtOH/HCl (20 ml) is refluxed for 2 hours. The solvent is then evaporated under vacuum and the residue diluted with H2O. The resulting aqueous solution is washed with CHCl3, basified with conc. NH4OH and the precipitate extracted with CHCl3. The combined organic extracts are dried over Na2SO4 and concentrated to give the product as a pale yellow solid (0.45 g, 64% yield, m.p. 94-96° C.). 1H-NMR (CDCl3): 3.14 (s, 2H), 5.04 (br s, 2H), 6.92-7.10 (m, 3H). MS (ESI): m/z 249 (M+H+).

WORKUP

后处理

  1. customThe solvent is then evaporated under vacuum
  2. additionthe residue diluted with H2O
  3. washThe resulting aqueous solution is washed with CHCl3
  4. extractionthe precipitate extracted with CHCl3
  5. dry with materialThe combined organic extracts are dried over Na2SO4
  6. concentrationconcentrated