Mitoxantrone hydrochloride synthesis
- Product Name:Mitoxantrone hydrochloride
- CAS Number:70476-82-3
- Molecular formula:C22H30Cl2N4O6
- Molecular Weight:517.4028
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70476-82-3
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Yield:70476-82-3 6.4 g
Reaction Conditions:
with hydrogenchloride in water; pH=Ca. 2.8 - 3 at 52 - 60; for 0.5 h;Inert atmosphere;Temperature;
Steps:
1-3 Example 3 Preparation of mitoxantrone hydrochloride 1.25 hydrate (ω type)
In a 500 ml three-necked flask, add 10 g of mitoxantrone, 80 ml of water, protect with nitrogen, stir, and add about 5.8 ml of 8 M hydrochloric acid dropwise at room temperature. If the pH of the solution exceeds 3 during the reaction,Then use 8M hydrochloric acid solution to adjust the solution pH to about 2.8, and then stir at 52-60 ° C.Add an appropriate amount of water, stir until completely dissolved, continue stirring for 0.5 hours, then add 50ml of methanol,120ml of absolute ethanol, stored below 0 ° C, after the precipitation is fully analyzed, suction filtration,Wash twice with a small amount of methanol, suction filter, and place the obtained solid in a flask.Add an appropriate amount of water to heat and stir to dissolve, and then use about 50ml of ethanol,Approximately 160 ml of isopropyl alcohol is used as a crystallization solvent for recrystallization.After the crystals were fully analyzed, the solution was filtered with suction. The solid was washed with a small amount of methanol and filtered with suction.The obtained solid was thinned and dried in an oven at 35 ° C. for about 5 hours to obtain 6.4 g of a blue-black crystalline solid.
References:
Liu Li CN110551038, 2019, A Location in patent:Paragraph 0085-0090
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70476-82-3
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