3-Nitrobenzenesulfonyl chloride → (2S,4R)-4-(3-Nitro-benzenesulfonyloxy)-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester

(2S,4R)-4-Hydroxy-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (5.0 g) was dissolved in DCM (50 mL) and 3-nitrobenzenesulfonyl chloride (4.8 g) was added. This solution was cooled to 5° C. and the TEA (8.52 mL) was carefully added. The reaction mixture was stirred at 25° C. for 18 h. The reaction mixture was then extracted with 0.1 N aqueous HCl (50 mL) and aqueous Na2CO3 (50 mL) and brine (50 mL). The organic layer was dried over Na2SO4, filtrated and evaporated to dryness to yield a light brown amorphous solid (9.05 g). MS: m/z=431.4 [M+H]+.

1. extractionThe reaction mixture was then extracted with 0.1 N aqueous HCl (50 mL) and aqueous Na2CO3 (50 mL) and brine (50 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltrated
4. customevaporated to dryness

ORDレコード

ord-ed6f79568ea1451898ce3a8046113a50

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524710B2