3-AMinopyrrolidine-3-carboxylic acid hydrochloride synthesis

Yield:-

Reaction Conditions:

with hydrogen;5% Pd(II)/C(eggshell) in methanol;water; under 3800.26 Torr; for 24 h;

Steps:

1.4

The crude product 3 above was dissolved in the mixture of Dl water and methanol (2mL/100mL). Pd/C powder (5%, 1.8g) was introduced and the reaction system was degassed. Then hydrogen gas was applied to the reaction system as 5 atm. The reaction was stirred at room temperature vigorously for 24 h. The pressure was released and the solid in the reaction mixture was filtered off. The crude product was obtained after removed most of the solvent. Strong acidic ion exchange resin (Amberjet 1200 H from Rohmhaas) was used to separate pure cucurbitine in neutral form with 5% ammonia water as eluent. Recrystalization by EtOH/H₂0 under pH =4~5 afforded its pure mono-hydrochloride salt. Yield 70% (two steps).

References:

WO2011/91548,2011,A1 Location in patent:Page/Page column 9