反应详情

4.2 g of (2S,4S)-4-Phenyl-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (13.75 mmol) in 30 ml tetrahydrofuran were slowly added to a suspension of 0.27 g of lithium aluminium hydride in 50 ml tetrahydrofurane. Stirring was continued for 5 h at 0-5° C. and for 14 h at room temperature. For workup, a mixture of tetrahydrofurane/water (1:1) was slowly added to the reaction mixture at 0° C. The solvent was then evaporated under reduced pressure, water was added and the pH was adjusted to about 5 with 20% aqueous citric acid. The aqueous phase was extracted four times with ethyl acetate, the organic layers were combined, dried over magnesium sulphate, filtered, and the solvent was removed under reduced pressure to yield 3.85 of product.

1. additionwas slowly added to the reaction mixture at 0° C
2. customThe solvent was then evaporated under reduced pressure, water
3. additionwas added
4. extractionThe aqueous phase was extracted four times with ethyl acetate
5. dry with materialdried over magnesium sulphate
6. filtrationfiltered
7. customthe solvent was removed under reduced pressure
8. customto yield 3.85 of product