反应详情

1.94 g (3 mmol) of D-Pro-Val-MeVal-Pro-Pro-NHBn×HCl was dissolved in 30 ml methanol. To this solution was then added 0.3 g 10% Pd/charcoal and 1.5 ml aqueous formaldehyde solution and the reaction mixture was hydrogenated. Following filtration and evaporation of the solvents, the resulting residue was dissolved in water, adjusted to pH 2 and extracted twice with diethyl ether and several additional times with dichloromethane. The aqueous phase was adjusted to pH 9-10 and extracted twice with dichloromethane. The organic extracts were dried over sodium sulfate and evaporated to dryness. The residue was crystallized as the hydrochloride salt to give 0.5 g of the desired product which was characterized by fast atom bombardment mass spectrometry ([M+H]+=625).

1. filtrationfiltration and evaporation of the solvents
2. dissolutionthe resulting residue was dissolved in water
3. extractionextracted twice with diethyl ether and several additional times with dichloromethane
4. extractionextracted twice with dichloromethane
5. dry with materialThe organic extracts were dried over sodium sulfate
6. customevaporated to dryness
7. customThe residue was crystallized as the hydrochloride salt