반응 #5164

반응 방정식

sodium bicarbonate

dioxane

hydrogen chloride

(2S, 4S)-1-(t-butoxycarbonyl)-2-carbamoyl-4-(4-methoxybenzylthio)pyrrolidine

→

title compound

수율 97.5%

(2S, 4S)-2-Carbamoyl-4-(4-methoxybenzylthio)-pyrrolidine

수율 97.5%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도cooling
2. 2
   추출was extracted with ethyl acetate
3. 3
   세척The extract was washed with an aqueous solution of sodium chloride
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타The solvent was then removed by distillation under reduced pressure

실험 절차

1.92 g of (2S, 4S)-1-(t-butoxycarbonyl)-2-carbamoyl-4-(4-methoxybenzylthio)pyrrolidine [prepared as described in step (4) above] was dissolved in 25 ml of ethyl acetate, and 26.2 ml of a 4N dioxane solution of hydrogen chloride were added to the solution, whilst ice-cooling. The mixture was then stirred at 0° to 5° C. for 2 hours and at room temperature for 30 minutes. At the end of this time, it was poured into a saturated aqueous solution of sodium bicarbonate, to make it weakly basic, and was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give 1.36 g of the title compound as a powder, melting at 120°-121° C.

출처