Triethylamine → 2-[3-(2-Oxo-1-pyrrolidinyl)phenyl]ethyl methanesulfonate

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).

1. washwashed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL)
2. dry with materialThe organic layer was dried over sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe crude was purified by flash chromatography on silica gel
5. washeluting with ethyl acetate-cyclohexane (50:50)

ORDレコード

ord-e43dbf51330b477594329fda39fed113

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07732600B2