反応 #4220

反応方程式

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

収率 65.0%

溶媒

ethanol

反応条件

後処理

1. 1
   濃縮The mixture was then concentrated
2. 2
   温度the ethyl acetate mixture was heated
3. 3
   温度It was then cooled in an ice bath
4. 4
   ろ過the solid was filtered off
5. 5
   洗浄rinsed with ethyl acetate
6. 6
   濃縮The filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   ろ過The precipitate was filtered off
9. 9
   洗浄rinsed with ether
10. 10
    その他the free base was obtained

実験手順

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.

出典