Reaktion #1175139

Reaktionsgleichung

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

Ausbeute 52.0%

Lösungsmittel

toluene

dimethyl sulphoxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 6 hours
3. 3
   workup.ADDITION2 g of silica gel were added to the reaction mixture and it
4. 4
   Filtrationwas then filtered
5. 5
   workup.ADDITION75 ml of semi-concentrated hydrochloric acid were added to the filtrate
6. 6
   Sonstigethe crystals which separated out
7. 7
   Filtrationthereby 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
   Filtrationfiltered off with suction
10. 10
    Waschenwashed with water to neutrality

Vorschrift

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.

Quelle