反应详情

温度

0 °C

A mixture of 11.2 g of (2S,4R)-1-(tert-butoxycarbonyl)-4-hydroxy-2-pyrrolidinecarboxylic acid in 50 ml of DCM is cooled to 0° C., 8.45 ml of DIPEA and then 21.2 g of BOP are added and the resulting mixture is stirred for 10 minutes. Dimethylamine gas is then added by sparging and the mixture is stirred for 3 hours at RT. The reaction mixture is partially concentrated under vacuum to a volume of 20 ml and an insoluble material is filtered off. The filtrate is chromatographed on silica gel, eluting with a DCM/MeOH mixture (94/6; v/v) and the product obtained is re-chromatographed on alumina, eluting with a DCM/MeOH mixture (96/4; v/v). 11.1 g of the expected product are obtained.

1. customby sparging
2. stirringthe mixture is stirred for 3 hours at RT
3. concentrationThe reaction mixture is partially concentrated under vacuum to a volume of 20 ml
4. filtrationan insoluble material is filtered off
5. customThe filtrate is chromatographed on silica gel
6. washeluting with a DCM/MeOH mixture (94/6; v/v)
7. customthe product obtained
8. customis re-chromatographed on alumina
9. washeluting with a DCM/MeOH mixture (96/4; v/v)