반응 #1470449
ord-69ceff90975f474ab36aaf24f94a7448
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후처리
- 1workup.STIRRINGthe mixture is agitated for a further 3 days at 20° C
- 2workup.ADDITIONare added
- 3workup.WAITAfter 18 hours' agitation at a temperature of 30° C.
- 4workup.DISTILLATIONthe solvents are distilled off
- 5세척The organic phase is washed twice with water and once with concentrated aqueous sodium chloride solution
- 6건조After the organic phase has been dried over sodium sulfate, it
- 7workup.ADDITIONis treated with activated charcoal
- 8여과filtered
- 9기타evaporated to dryness
- 10기타After recrystallization from a little diisopropylether
실험 절차
To a solution of 12.5 g (28.4 mmol) 2-(bis-methylsulfanylmethylene)-1 -cyclopropyl-3-(2-methanesulfonyl-4-trifluoromethylphenyl)propane-1,3-dione in 80 ml dichloromethane, 140 ml each of ethanol, 2.82 g (39.8 mmol) hydroxylamine hydrochloride and 3.4 g (41.2 mmol) anhydrous sodium acetate is successively added. The reaction mixture is then agitated for 48 hours at a temperature of 20° C. Then 50 ml dichloromethane, 50 ml ethanol, 1.4 g hydroxylamine hydrochloride and 1.7 g anhydrous sodium acetate are added, and the mixture is agitated for a further 3 days at 20° C. The reaction mixture is subsequently heated to a temperature of 30° C., and 2.8 g hydroxylamine hydrochloride and 3.4 g sodium acetate are added. After 18 hours' agitation at a temperature of 30° C., the solvents are distilled off and the residue taken up in 300 ml ethyl acetate. The organic phase is washed twice with water and once with concentrated aqueous sodium chloride solution. After the organic phase has been dried over sodium sulfate, it is treated with activated charcoal, filtered and evaporated to dryness. After recrystallization from a little diisopropylether, 10.7 g 5-cyclopropyl-3-methylsulfanyl-4-(2-methanesulfonyl-4-trifluoromethylbenzoyl)isoxazole is obtained in the form of crystalline solid matter with a melting point of 145-146° C.