Tripteryglide cinnamate derivatives and preparation method and use thereof
A technology of tripterine and cinnamate, which is applied in the direction of pharmaceutical formulations, drug combinations, steroids, etc., and can solve the problems that the activity needs to be improved
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0038] Embodiment 1: the preparation of intermediate II-1
[0039] 2-Bromoethanol (1mM, 1eq, 70.9μl) was dissolved in 6mL of DCM, and cinnamic acid (1.2mM, 1.2eq, 177.6mg), EDCI (1.5mM, 1.5eq, 287.6mg) and DMAP ( 0.5mM, 0.5eq, 61.1mg), stirred at room temperature for 7 hours, concentrated under reduced pressure and dissolved in DCM, followed by 5% NaHCO 3 The organic layer was washed with aqueous solution and saturated NaCl solution, dried over anhydrous sodium sulfate, spin-dried, and purified by silica gel column chromatography (PE / EA=16:1) to obtain 137.2 mg of white solid with a yield of 54%.
[0040] ESI-MS: Bromine isotope characteristic peaks 255.0, 257.0 [M+H] + .
[0041] The reaction formula is as follows:
[0042]
Embodiment 2
[0043] Embodiment 2: the synthesis of I-1
[0044] Dissolve 45.0mg (0.1mM, 1.0eq) tripterine in 2ml DMF, add 42.0mg NaHCO 3 (0.5mM, 5.0eq), stirred for 7h, added 76.2mg (0.3mM, 3.0eq) of intermediate II-1, and heated to reflux at 60°C. Until TLC detection shows that the reaction is complete, add 50ml CH 2 Cl 2 Dilute, extract with water, discard the aqueous layer, wash the organic layer with saturated NaCl, dry over anhydrous sodium sulfate, filter with suction, evaporate the solvent to dryness, and purify by column chromatography (PE / EA=6:1) to obtain 34.3mg, yield 55 %.
[0045] ESI-MS: 647.3 [M+Na] + .
[0046] 1 H-NMR (300MHz, CDCl 3 , TMS), δppm: 0.58(3H,s), 1.11(3H,s), 1.22(3H,s), 1.26(3H,s), 1.43(3H,s), 2.21(3H,s), 4.08- 4.12(1H,m),4.30-4.46(3H,m),6.26(1H,d,J=7.1Hz),6.44(1H,d,J=16.0Hz),6.52(1H,s),6.95(1H ,d,J=7.1Hz),7.43(3H,m),7.55(2H,m),7.72(1H,d,J=16.1Hz).
[0047]
Embodiment 3
[0048] Embodiment 3: the preparation of intermediate II-2
[0049] The 2-bromoethanol in Example 1 was replaced with 3-bromo-1-propanol (1mM, 1eq, 90.4μl), and other conditions remained unchanged, to obtain 141.5mg of white solid II-2 with a yield of 52.8%.
[0050] ESI-MS: Bromine isotope characteristic peaks 269.0, 271.0 [M+H] + .
[0051] The reaction formula is as follows:
[0052]
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


