反応 #539677

反応方程式

4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-trifluoromethyl benzoic acid methyl ester

sodium hydroxide

→

aimed product

収率 87.5%

4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-trifluoromethyl benzoic acid

収率 87.5%

溶媒

methanol

water

water

反応条件

後処理

1. 1
   workup.ADDITIONwas added in the reaction mixture
2. 2
   洗浄washed with 5 ml of toluene, aqueous phase
3. 3
   その他was collected
4. 4
   抽出extracted with ethyl acetate (20 ml×2)
5. 5
   洗浄The organic phase was washed with water
6. 6
   乾燥dried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

実験手順

In a solution of 0.40 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-trifluoromethyl benzoic acid methyl ester in 5 ml of methanol, a solution of 0.10 g of sodium hydroxide in 2 ml of water was added, and stirred at room temperature for 18 hours. After the completion of the reaction, 10 ml of water was added in the reaction mixture, washed with 5 ml of toluene, aqueous phase was collected, adjusted to pH 1 to 2 with concentrated hydrochloric acid and then extracted with ethyl acetate (20 ml×2). The organic phase was washed with water, dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure to obtain 0.34 g of the aimed product as pale yellow resinous substance. The resulting product was used as such without purification for the next step.

出典