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ChemicalBook CAS DataBase List Pixantrone Impurity B
144510-94-1

Pixantrone Impurity B synthesis

7synthesis methods
-

Yield:144510-94-1 80%

Reaction Conditions:

with potassium carbonate in 1-methyl-pyrrolidin-2-one at 60; for 5 h;Temperature;

Steps:

1 Embodiment 1 6,9-bis-[(2-aminoethyl)amino]benzo[g] isoquinoline-5,10-maleic acid salt, according to the following process step synthesis:k

2.0 g (0.05 mol, leq.) of the first intermediate prepared in the previous step, 16.0 g (0 lmol, 2 eq.) N-t-butoxy carbonyl ethylenediamine, 6.9 g (0.05 Mol, leq.) potassium carbonate and 60 mL of N-methylpyrone (1: 2: 1 in the first intermediate, N-tert-butoxy carbonylethylenediamine and potassium carbonate), heated to 60 °C for 5 h, and the reaction was carried out by HPLC. The second solution was slightly cooled and the second solution was slowly poured into 240 mL of deionized water (the first intermediate and the deionized group), and the second solution was slowly cooled and the second solution was slowly poured into 240 mL of deionized water Water weight ratio of 1:20), stirring a large amount of blue-colored second solid, filtered at room temperature, the filter cake was washed three times with water, and then mixed with 120 mL of methanol and dichloromethane (V / V = l: l) The solvent was recrystallized and filtered at 0-5 °C to give a second intermediate, 80% yield, 99.5% pure.

References:

CN106366036,2017,A Location in patent:Paragraph 0059