反应详情

6.2 g of HOBT and then 9.45 g of DCC are added at RT to a solution of 10 g of (2S)-1-(tert-butoxycarbonyl)piperidine-2-carboxylic acid (commercial) in 130 ml of DCM, and the mixture is left stirring for 1 hour. The reaction mixture is cooled on an ice bath, dimethylamine gas is added by bubbling for two times 10 minutes and the mixture is then left stirring overnight at RT. An insoluble material is filtered off and the filtrate is concentrated under vacuum. The residue is chromatographed on silica gel, eluting with a gradient of a DCM/MeOH mixture of from (98/2; v/v) to (96/4; v/v). The product obtained is taken up in ether and the precipitate is spin-filtered off. 8.5 g of the expected product are obtained.

1. waitthe mixture is left
2. temperatureThe reaction mixture is cooled on an ice bath
3. customby bubbling for two times 10 minutes
4. waitthe mixture is then left
5. stirringstirring overnight at RT
6. filtrationAn insoluble material is filtered off
7. concentrationthe filtrate is concentrated under vacuum
8. customThe residue is chromatographed on silica gel
9. washeluting with a gradient of a DCM/MeOH mixture of from (98/2; v/v) to (96/4; v/v)
10. customThe product obtained
11. filtrationthe precipitate is spin-filtered off