反应详情

268.3 g (0.79 mol) of crude 1-bromo-4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one were dissolved in 2 l of absolute acetonitrile. 190 g (2.7 mol) of 1,2,4-triazole were added thereto and the mixture was heated for 20 hours under reflux. It was then concentrated by distilling off the solvent in vacuo and the residue was taken up in 1,000 ml of methylene chloride. The mixture was washed three times with 250 ml of water at a time, dried over sodium sulphate and again concentrated in vacuo. The oil which remained was dissolved in 1,000 ml of acetone and a solution of 140 g (0.48 mol) of naphthalenedisulphonic acid in 500 ml of acetone was added. After 30 minutes, the resulting precipitate was filtered off. 285 g (76.6% of theory) of 4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate of melting point 245° C. (with decomposition) were obtained.

1. temperaturethe mixture was heated for 20 hours
2. temperatureunder reflux
3. concentrationIt was then concentrated
4. distillationby distilling off the solvent in vacuo
5. washThe mixture was washed three times with 250 ml of water at a time
6. dry with materialdried over sodium sulphate
7. concentrationagain concentrated in vacuo
8. dissolutionThe oil which remained was dissolved in 1,000 ml of acetone
9. filtrationthe resulting precipitate was filtered off