تفاعل #4220

معادلة التفاعل

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-1yl)butan-2-ol

المردود 65.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   تركيزThe mixture was then concentrated
2. 2
   درجة الحرارةthe ethyl acetate mixture was heated
3. 3
   درجة الحرارةIt was then cooled in an ice bath
4. 4
   ترشيحthe solid was filtered off
5. 5
   غسيلrinsed with ethyl acetate
6. 6
   تركيزThe filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   ترشيحThe precipitate was filtered off
9. 9
   غسيلrinsed with ether
10. 10
    أخرىthe free base was obtained

الإجراء التجريبي

72.15 g (0.3 mole) 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-1yl)butan-2-ol of melting point 84°-87° C. were obtained.

المصدر