Trifluoroacetic acid → Phthalimide

3-Trifluoromethylphenylsulfonyl chloride (1.96 g, 8.00 mmol) was added to a solution of (S)-2-(pyrrolidin-3-yloxy)isoindoline-1,3-dione) trifluoroacetic acid salt (2.77 g, 8.00 mmol) and N,N-diisopropylethylamine (3.10 g, 24.0 mmol) in CH2Cl2 (50 ml) and stirred at room temperature for 4 hours. The reaction mixture was washed with aqueous 1 N HCl solution (50 ml×2), H2O (50 ml×3) and brine (50 ml), dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by column chromatography (ethyl acetate/petroleum ether: 12.5/87.5 to 50/50) to give (S)-2-(1-(3-trifluoromethyl)phenylsulfonyl)pyrrolidin-3-yloxy)isoindoline-1,3-dione (1.87 g, 53%) as a white solid.

1. washThe reaction mixture was washed with aqueous 1 N HCl solution (50 ml×2), H2O (50 ml×3) and brine (50 ml)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography (ethyl acetate/petroleum ether: 12.5/87.5 to 50/50)

ORDレコード

ord-dfad427633e34ed9a25b4fd826047009

出典データセット

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08518934B2