반응 #214063

반응 방정식

1-(4-chlorophenoxy)-1-(imidazol-1-yl)-3,3-dimethyl-4-chlorobutan-2-ol

dichloroacetyl chloride

→

1-(4-chlorophenoxy)-1-(imidazol-1-yl)-2-dichloroacetoxy-3,3-dimethyl-4-chloro-butane

수율 29.0%

반응 조건

후처리

1. 1
   workup.DISTILLATIONexcess dichloroacetyl chloride was distilled off in vacuo
2. 2
   기타the organic phase was separated off
3. 3
   세척washed with 200 ml of water
4. 4
   건조dried over sodium sulphate
5. 5
   workup.DISTILLATIONThe solvent was distilled off
6. 6
   기타After leaving the mixture
7. 7
   workup.WAITto stand for several hours
8. 8
   기타colorless crystals precipitated

실험 절차

19.8 g (0.06 mol) of 1-(4-chlorophenoxy)-1-(imidazol-1-yl)-3,3-dimethyl-4-chlorobutan-2-ol were added to 200 ml of dichloroacetyl chloride at 0° C. The mixture was stirred at room temperature for 24 hours and excess dichloroacetyl chloride was distilled off in vacuo. The oil which remained was taken up in 400 ml of methylene chloride, the methylene chloride mixture was neutralized with 500 ml of aqueous sodium bicarbonate solution, the organic phase was separated off, washed with 200 ml of water and dried over sodium sulphate. The solvent was distilled off and the residue was taken up in 200 ml of diisopropyl ether. After leaving the mixture to stand for several hours, colorless crystals precipitated. 7.5 g (29% of theory) of 1-(4-chlorophenoxy)-1-(imidazol-1-yl)-2-dichloroacetoxy-3,3-dimethyl-4-chloro-butane of melting point 108°-110° C. were obtained.

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