Cinepazide medicinal composition with high safety, preparation method and application thereof
A technology of cinepazide and composition, which is applied in the field of cinepazide pharmaceutical composition and its preparation, and can solve problems such as not effectively reducing
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[0066] Example 1 Preparation of cinepazide nitrogen oxide
[0067] Dissolve 2 grams of cinepazide in 100 ml of dichloromethane, add 10 grams of peroxyacetic acid, stir until the reaction is complete, filter, spin-dry the filtrate, recrystallize with ethanol, and then freeze-dry to obtain 0.52 g of cinepazide Special nitrogen oxides. HPLC peak area normalization method shows that its content is not less than 98%.
[0068] 1 H NMR(300MHz, CDCl 3 )δ(ppm): 7.615(d, 1H) 6.731(d, 1H) 6.610(s, 2H) 3.801(m, 1H), 4.012(m, 2H), 4.131(m, 1H) 4.674(d, 1H) , 4.278 (d, 1H) 3.907 (s, 6H) 3.882 (s, 3H) 3.251 (d, 2H), 3.589 (d, 2H) 3.504 (t, 2H) 4.137 (t, 2H) 1.914 (m, 2H) , 2.015 (m, 2H)
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[0069] Example 2 Preparation of Cinepezide Nitrogen Oxide
[0070] Dissolve 2 g of cinepazide in 100 ml of methanol, add 5 g of peroxybenzoic acid, stir until the reaction is complete, filter, spin dry the filtrate, separate with a preparative high performance liquid phase, the mobile phase is methanol-water, gradient wash After removing and receiving the product fraction, 0.3 g of cinepazide nitrogen oxide is obtained. HPLC peak area normalization method shows that its content is not less than 99%.
[0071] 1H NMR (600MHz, DMSO) δ (ppm): 7.492 (d, 1H) 7.238 (d, 1H) 7.060 (s, 2H) 4.306 (dd, 2H), 4.090 (s, 2H), 3.913 (m, 1H) 3.835 (s, 6H), 3.723 (m, 1H) 3.689 (s, 3H) 3.641 (m, 3H), 3.489 (s, 1H) 3.311 (t, 2H) 3.186 (m, 2H) 1.853 (m, 2H) , 1.776 (m, 2H)
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[0072] Example 3 Preparation of Cinepezide Nitrogen Oxide
[0073] Dissolve 5 g of Cinepazide maleate in 25 ml of water, add 25 ml of 25% hydrogen peroxide, stir at room temperature for 5 days, separate with preparative high performance liquid phase, mobile phase acetonitrile-water, gradient elution, receive The fraction of the product yields 500 mg of cinepazide nitrogen oxide. HPLC peak area normalization method shows that its content is not less than 99%.
[0074] MS(LC-MS)=434.2(M+H + ), 867.5(2M+H + ).
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