TOPOTECANACETATE synthesis
- Product Name:TOPOTECANACETATE
- CAS Number:123948-88-9
- Molecular formula:C25H27N3O7
- Molecular Weight:481.51
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Yield:-
Reaction Conditions:
in water at 45.3; for 2.41667 h;
Steps:
2
EXAMPLE 2 Preparation of Topotecan Acetate of Formula V 0.3 Kg of 10-hydroxy camptothecin (Formula IV) prepared according to Example-1 was suspended in 6 L of acetic acid and stirred for 5 minutes. The obtained solution was charged into a reactor and stirred for 20 minutes. 0.51 L of a 40% aqueous solution of dimethyl amine and 0.078 L of a 37% of aqueous solution of formaldehyde were charged into the reactor, the temperature raised to 45.3° C. and the reaction mixture stirred for 2 hours at 45.3° C. The reaction solution was allowed to cool to 34.8° C. and then cooled to 27.5° C. 42 L of acetone was charged into above reaction solution and stirred for 1 hour at 27.5° C. for complete precipitation. The formed solid was filtered and the reactor rinsed with 1.5 L of acetone. The wet solid was washed with the rinsing and then washed with 0.3 L of 1-propanol. The resultant solid was suction dried for 20 minutes and then dried for 5 hours at 52° C. under a vacuum of 690 mm Hg to afford 330 g of title compound having a purity by HPLC of about 98.9%.
References:
US2007/149783,2007,A1 Location in patent:Page/Page column title page; 7
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