HRID1966057
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent is then evaporated under vacuum
- additionthe residue diluted with H2O
- washThe resulting aqueous solution is washed with CHCl3
- extractionthe precipitate extracted with CHCl3
- dry with materialThe combined organic extracts are dried over Na2SO4
- concentrationconcentrated