Icaritin analogue and its preparation method and application
The technology of icariin and its analogs is applied in the field of development and application of medicinal compounds, and can solve the problems of general anti-tumor effect of icariin and limited clinical application, etc.
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Embodiment 1
[0080] Synthesis of 8-((diethylamino)methyl)-2-(2,4-dimethoxyphenyl)-3,7-dihydroxy-4H-chroman-4-one (Ⅰ-1):
[0081]
[0082] To a solution of 2-(2,4-dimethoxyphenyl)-3,7-dihydroxy-4H-chroman-4-one (150 mg, 0.48 mmol) in EtOH (5 mL) was added formalin ( 37%, 1.3eq) and diethylamine (65 μL, 0.63mmol). The reaction mixture was stirred at 80°C for about 8 hours. The solution was then cooled to room temperature and the precipitated solid was collected by filtration, washed with methanol and recrystallized from ethanol to give a yellow solid in 80% yield. 1 H NMR (300 MHz, Chloroform- d ) δ 8.04 (d, J = 8.9 Hz, 1H), 7.56 (d, J = 8.5 Hz, 1H), 7.26 (s, 1H), 6.86 (d, J = 8.8 Hz,1H), 6.64 (dd, J = 8.4, 2.4 Hz, 1H), 6.60 (d, J = 2.3 Hz, 1H), 4.07 (s, 2H), 3.88 (s, 3H), 3.85 (s, 3H), 2.70 (q, J = 7.2 Hz, 4H), 1.16 (t, J = 7.2 Hz,6H).
Embodiment 2
[0084] Synthesis of 2-(2,4-dimethoxyphenyl)-3,7-dihydroxy-8-(pyrrolidin-1-ylmethyl)-4H-chroman-4-one (Ⅰ-2) :
[0085]
[0086] Referring to the synthetic method of compound (I-1), the yield was 70%. 1 H NMR (300 MHz, Chloroform- d ) δ 8.05 (d, J = 8.9 Hz, 1H), 7.56 (d, J = 8.4 Hz, 1H), 6.87 (d, J = 8.8 Hz, 1H),6.64 (dd, J = 8.5, 2.4 Hz, 1H), 6.60 (d, J = 2.3 Hz, 1H), 4.14 (s, 2H), 3.88(s, 3H), 3.86 (s, 3H), 2.73 (s, 4H), 1.90 (m, J = 3.5 Hz, 4H).
Embodiment 3
[0088] Synthesis of 2-(2,4-dimethoxyphenyl)-3,7-dihydroxy-8-(morpholinomethyl)-4H-chroman-4-one (Ⅰ-3):
[0089]
[0090] Referring to the synthetic method of compound (I-1), the yield was 85%. 1 H NMR (300 MHz, Chloroform- d ) δ 8.08 (d, J = 8.9 Hz, 1H), 7.57 (dd, J = 8.4, 0.4 Hz, 1H), 6.89 (d, J = 8.9Hz, 1H), 6.64 (dd, J = 8.4, 2.3 Hz, 1H), 6.61 (d, J = 2.3 Hz, 1H), 4.02 (s,2H), 3.89 (s, 3H), 3.87 (s, 3H), 3.80 (s, 4H), 2.65 (s, 4H).
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