Irinotecan hydrochloride trihydrate synthesis

Yield:136572-09-3 87%

Reaction Conditions:

with hydrogenchloride;water in ethanol at 75 - 80;

Steps:

3
Irinotecan HCl (4.8 g), water (30 ml), ethanol (10 ml) and 5 % HCl (0.3 ml) were charged. The mixture was heated to 75-80 °C and stirred until all dissolved. The solution was cooled to 65 ⁰C and seed crystals were added. The solution was cooled in 10 hours to 50 °C and in 10 hours to 20 ⁰C. The crystalline compound was filtered and washed with water ( 16 ml) .The product was dried under normal pressure at room temperature.The yield of irinotecan HCl 3H2O was 4.6 g (87 %).The HPLC-purity was 99.9 %. Based on X-ray and IR analysis the product is form b as defined in WO 03/074527. The average length of the crystals was 50 μm -200 μm by microscopic analysis.

References:

FERMION OY WO2006/84941, 2006, A2 Location in patent:Page/Page column 6

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