Reaktion #214420

Reaktionsgleichung

naphthalenedisulphonic acid

1-bromo-4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one

1,2,4-triazole

→

4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate

Ausbeute 192.6%

Lösungsmittel

acetone

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated for 20 hours
2. 2
   Temperaturunder reflux
3. 3
   EinengenIt was then concentrated
4. 4
   workup.DISTILLATIONby distilling off the solvent in vacuo
5. 5
   WaschenThe mixture was washed three times with 250 ml of water at a time
6. 6
   Trocknendried over sodium sulphate
7. 7
   Einengenagain concentrated in vacuo
8. 8
   workup.DISSOLUTIONThe oil which remained was dissolved in 1,000 ml of acetone
9. 9
   Filtrationthe resulting precipitate was filtered off

Vorschrift

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.

Quelle