Реакция #214420

Уравнение реакции

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

Выход 192.6%

Растворители

acetone

acetonitrile

Условия реакции

Обработка

1. 1
   Температураthe mixture was heated for 20 hours
2. 2
   Температураunder reflux
3. 3
   КонцентрированиеIt was then concentrated
4. 4
   workup.DISTILLATIONby distilling off the solvent in vacuo
5. 5
   ПромывкаThe mixture was washed three times with 250 ml of water at a time
6. 6
   Сушкаdried over sodium sulphate
7. 7
   Концентрированиеagain concentrated in vacuo
8. 8
   workup.DISSOLUTIONThe oil which remained was dissolved in 1,000 ml of acetone
9. 9
   Фильтрацияthe resulting precipitate was filtered off

Методика

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.

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