Method for purifying bendamustine hydrochloride
A technology of bendamustine hydrochloride and a purification method, which is applied in the field of purification of bendamustine hydrochloride, and achieves the effects of simple process, good product quality and high yield
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Embodiment 1
[0013] 10 grams of bendamustine hydrochloride crude product (containing HP1 1.8%) was placed in a flask, and 50 milliliters of 0.01N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to 0°C for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 8.6 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.06%, other impurity: 0.08%, Water content: 0.9%).
[0014] 1 H-NMR (DMSO-d6, 400MHz): δ7.70(d, 1H), 7.07(d, 1H), 6.88(s, 1H), 3.87(s, 3H), 3.74(m, 8H), 3.14( t, 2H), 2.38(t, 2H), 1.99(m, 2H). Elemental analysis C 16 h 22 Cl 3 N 3 o 2 Calculated (%): C, 48.68; H, 5.62; N, 10.65; Cl, 26.95; found (%): C, 47.96; H, 5.64; N, 10.43; Cl, 26.00.
Embodiment 2
[0016] 10 grams of crude bendamustine hydrochloride (containing 1.8% HP1) was placed in a flask, and 50 milliliters of 0.1N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to room temperature for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 8.1 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.07%, other impurity: 0.06%, Water content: 0.7%).
Embodiment 3
[0018] 10 grams of bendamustine hydrochloride crude product (containing HP1 1.8%) was placed in a flask, and 50 milliliters of 1N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to 35°C for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 7.2 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.05%, other impurity: 0.05%, Water content: 0.9%).
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