反応 #77814

反応方程式

methanol

methyl 3-[4-methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionate

sodium hydroxide

→

aimed product

収率 74.9%

3-[4-Methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionic acid

収率 74.9%

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   洗浄washed with diethyl ether
3. 3
   抽出was extracted with methylene chloride
4. 4
   洗浄The organic layer was washed with water and saturated brine in sequence
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONSolvent was distilled off under reduced pressure
7. 7
   その他the crystals obtained
8. 8
   その他were recrystallized from diethyl ether-ethyl acetate

実験手順

Into 6 ml of methanol were dissolved 300 mg of methyl 3-[4-methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionate, 0.7 ml of 1 mol/l aqueous solution of sodium hydroxide were added, and the mixture was stirred for 1 hour at 50° C. The reaction mixture was poured into water and washed with diethyl ether. The aqueous layer was adjusted to pH value of 1 to 2 with 2 mol/l aqueous solution of hydrochloric acid, which was extracted with methylene chloride. The organic layer was washed with water and saturated brine in sequence and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the crystals obtained were recrystallized from diethyl ether-ethyl acetate to obtain 218 mg of aimed product as colorless crystals.

出典