Реакция #458666

Уравнение реакции

2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane

1,2,4-triazole

ethyl acetate

→

2-(4-chlorophenoxy-methyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol

Выход 65.0%

Растворители

ethanol

Условия реакции

Обработка

1. 1
   КонцентрированиеThe mixture was then concentrated
2. 2
   Температураthe ethyl acetate mixture was heated
3. 3
   ТемператураIt was then cooled in an ice bath
4. 4
   Фильтрацияthe solid was filtered off
5. 5
   Промывкаrinsed with ethyl acetate
6. 6
   КонцентрированиеThe filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   ФильтрацияThe precipitate was filtered off
9. 9
   Промывкаrinsed with ether
10. 10
    Другоеthe free base was obtained

Методика

72.15 g (0.3 mols) of 2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane and 24.15 g (0.35 mole) of 1,2,4-triazole were heated under reflux in 120 ml of ethanol for 48 hours. The mixture was then concentrated, the residue was taken up in 200 ml of ethyl acetate and the ethyl acetate mixture was heated. It was then cooled in an ice bath and the solid was filtered off and rinsed with ethyl acetate. The filtrate was concentrated, the residue was dissolved in ether/hexane and the solution was gassed with hydrogen chloride. The precipitate was filtered off and rinsed with ether and the free base was obtained by adding ethyl acetate/1N sodium hydroxide solution. 60.2 g (65% of theory) of 2-(4-chlorophenoxy-methyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 84°-87° C. were obtained.

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