反应详情

1.48 g (3.7 mmol) of 1,4-dibenzyl-2-(1′-pyrrolidinocarbonyloxymethyl)piperazine are dissolved in 40 ml of absolute ethanol and 1 ml of 12N HCl in a 100 ml ground-necked round-bottomed flask. About 100 mg of palladium (10%) on charcoal are added thereto. The mixture is then placed under a hydrogen atmosphere, vigorously stirred and gentle heating is applied (40° C.). When the initial product has disappeared (the reaction program is monitored by thin-layer chromatography eluted with an MeOH/CH2Cl2 mixture (5/95 v/v), after neutralization of an aliquot with a few grains of NaHCO3), the solution is filtered on paper and the catalyst is rinsed several times with ethanol and water. The solvents are then evaporated off under vacuum. 1.04 g of 2-(1′-pyrrolidinocarbonyloxymethyl)piperazine hydrochloride are thus obtained and used in the following step without further purification. Yield: 98.3%. Rf=0.4 (80/20/2 v/v/v CHCl3/MeOH/NH4OH).

1. temperaturegentle heating
2. custom(40° C.)
3. washeluted with an MeOH/CH2Cl2 mixture (5/95 v/v)
4. filtrationafter neutralization of an aliquot with a few grains of NaHCO3), the solution is filtered on paper
5. washthe catalyst is rinsed several times with ethanol and water
6. customThe solvents are then evaporated off under vacuum