Реакция #1175139

Уравнение реакции

2-(4-chlorophenoxymethyl)-2-tert.-butyloxirane

1,2,4-triazole

potassium hydroxide

→

2-(4-chlorophenoxymethyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanol

Выход 52.0%

Растворители

toluene

dimethyl sulphoxide

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураunder reflux for 6 hours
3. 3
   workup.ADDITION2 g of silica gel were added to the reaction mixture and it
4. 4
   Фильтрацияwas then filtered
5. 5
   workup.ADDITION75 ml of semi-concentrated hydrochloric acid were added to the filtrate
6. 6
   Другоеthe crystals which separated out
7. 7
   Фильтрацияthereby were filtered off with suction
8. 8
   workup.ADDITIONThen 80 ml of water and aqueous sodium hydroxide solution were added to the crystalline solid so that the pH of the mixture
9. 9
   Фильтрацияfiltered off with suction
10. 10
    Промывкаwashed with water to neutrality

Методика

A mixture of 30 g of 2-(4-chlorophenoxymethyl)-2-tert.-butyloxirane, 9.8 g of 1,2,4-triazole and 1.2 g of solid potassium hydroxide in 70 ml of toluene and 7.5 ml of dimethyl sulphoxide was heated under reflux for 6 hours. After cooling to room temperature, 2 g of silica gel were added to the reaction mixture and it was then filtered. 75 ml of semi-concentrated hydrochloric acid were added to the filtrate, and the crystals which separated out thereby were filtered off with suction. Then 80 ml of water and aqueous sodium hydroxide solution were added to the crystalline solid so that the pH of the mixture was 13. It was stirred a further 2 hours at room temperature, then filtered off with suction and washed with water to neutrality. In this manner, 20 g (52% of theory) of 2-(4-chlorophenoxymethyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanol of melting point 84°-87° C. were obtained.

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