Hydrochloric Acid → n-(o-(3-Maleinimidobenzoyl)-2-hydroxyethyl)-1,2-diaminoethane dihydrochloride

Participants

Reaction Steps

6 g (11.93 mmol) of N-(O-(3-maleinimidobenzoyl)-2-hydroxyethyl)-N,N′-bis-tertiarybutyloxycarbonyl-1,2-diaminoethane are diluted with 60 ml (5 eq) of a 1 M solution of HCl in diethylether while stirring at room temperature. After 48 h of stirring at room temperature, the fine-crystallinic precipitate is suctioned off over a G4 glass frit, freed of the HCl residues through multiple washing with anhydrous ether and dried under a vacuum. Obtained are 3.0 g (7.98 mmol) of the product as a fine-powdery yellow solid, corresponding to 66.9% of the theoretically possible yield. Elementary analysis for C15H19N3O4Cl2 (375.9 g/mol); calculated: C: 47.89%, H: 5.05%, N: 11.17%, Cl: 18.86%; found: C: 46.97%, H: 5.42%, N: 10.03%, Cl: 17.63%.

Provenance & Evidence