반응 #78023

반응 방정식

HCl

N—(O—(3-maleinimidobenzoyl)-2-hydroxyethyl)-N,N′-bis-tertiarybutyloxycarbonyl-1,2-diaminoethane

HCl

→

N—(O—(3-maleinimidobenzoyl)-2-hydroxyethyl)-1,2-diaminoethane dihydrochloride

용매

—

solution

diethylether

반응 조건

후처리

1. 1
   workup.STIRRINGAfter 48 h of stirring at room temperature
2. 2
   세척through multiple washing with anhydrous ether
3. 3
   기타dried under a vacuum
4. 4
   기타Obtained

실험 절차

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 1M 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);

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