Реакция #1252886

Уравнение реакции

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

1,2,4-triazole

→

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 solution heated
3. 3
   ТемператураThe solution was thereafter cooled in an ice bath
4. 4
   Фильтрацияthe solid material was filtered off under suction
5. 5
   Промывкаwas washed with ethyl acetate
6. 6
   КонцентрированиеThe filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   workup.ADDITIONthe solution was treated with gaseous hydrogen chloride
9. 9
   ФильтрацияThe precipitate was filtered off under suction
10. 10
    Промывкаwashed with ether
11. 11
    Другоеthe free base was obtained by the addition of ethyl acetate/1N sodium hydroxide solution

Методика

72.15 g (0.3 mol) of 2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane and 24.15 g (0.35 mol) of 1,2,4-triazole were heated under reflux in 120 ml of ethanol for 48 hours. The mixture was then concentrated, and the residue was taken up in 200 ml of ethyl acetate and the solution heated. The solution was thereafter cooled in an ice bath, and the solid material was filtered off under suction and was washed with ethyl acetate. The filtrate was concentrated and the residue was dissolved in ether/hexane, and the solution was treated with gaseous hydrogen chloride. The precipitate was filtered off under suction and washed with ether, and the free base was obtained by the addition of 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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