반응 #44157

반응 방정식

Methanesulfonyl chloride

1-[3-(2-hydroxyethyl)phenyl]-2-pyrrolidinone

triethylamine

→

title compound

수율 93.0%

2-[3-(2-oxo-1-pyrrolidinyl)phenyl]ethyl methanesulfonate

수율 93.0%

용매

dichloromethane

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL)
2. 2
   건조The organic layer was dried over sodium sulfate
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The crude was purified by flash chromatography on silica gel
5. 5
   세척eluting with ethyl acetate-cyclohexane (50:50)

실험 절차

Methanesulfonyl chloride (0.124 mL) was added dropwise to a stirred solution of 1-[3-(2-hydroxyethyl)phenyl]-2-pyrrolidinone (0.30 g) and triethylamine (0.42 mL) in dichloromethane (10 mL) at room temperature under an inert atmosphere. The solution was stirred for 2 hours. The reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL), a saturated aqueous solution of sodium hydrogencarbonate (50 mL) and brine (50 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude was purified by flash chromatography on silica gel, eluting with ethyl acetate-cyclohexane (50:50) to afford the title compound in 93% yield (0.384 g).

출처