Indolizine heterocyclic nitrogen naphthoquinone derivatives as well as preparation method and anticancer use thereof
A technology of naphthoquinones and derivatives, which is applied in the field of preparation of cancer drugs, can solve the problem of unsatisfactory anti-tumor activity of camptothecin, and achieve the effect of low toxicity and strong inhibitory activity of normal cells
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0019] Example 1. Synthesis of Indenaza naphthoquinone derivatives NP1-A and NP1-B
[0020] Add 0.01mol of 6,7-dichloro-5,8-quinolinedione and 0.04mol of ethyl acetoacetate into 20-80ml of absolute ethanol, add 0.01-0.08mol of 3-fluoropyridine under stirring, reflux The reaction is carried out for 5 to 20 hours. Terminated, cooled, and solids were precipitated. Filtration, the obtained solid was separated by silica gel column chromatography, and a pair of indolizine aza naphthoquinone derivative isomers NP1-A and NP1-B were obtained at the same time.
[0021] NP1-A: 12% yield; m.p.=197-200°C; ESI: 339.0 (100%), 340.1 (20%) [M+1] + ; 1 H NMR (300MHz, CDCl 3 , TMS): δ9.64 (d, 1H, J=6.8Hz), 9.06 (dd, 1H, J=4.8, 1.6Hz), 8.54 (dd, 1H, J=8.0, 1.6Hz), 7.67 (dd, 1H, J=8.0, 4.8Hz), 7.16-7.06 (m, 2H), 4.54 (q, 2H, J=7.2Hz), 1.47 (t, 3H, J=7.2Hz).
[0022] NP1-B: 18% yield. m.p.=200-202°C; ESI: 339.0 (100%), 340.1 (20%) [M+1] + ; 1 H NMR (300MHz, CDCl 3 , TMS): δ9.49 (dd, 1H, J=...
Embodiment 2
[0025] Example 2. Synthesis of Indenaza naphthoquinone derivatives NP2-A and NP2-B
[0026] The method is the same as in Example 1, except that ethyl acetoacetate is replaced by nitroethane, and 3-fluoropyridine is replaced by pyridine, and a pair of indolizazine naphthoquinone derivative isomers NP2-A and NP2-A are obtained simultaneously. NP2-B.
[0027] NP2-A: 19% yield; m.p.=233°C; ESI: 263.3 (100%) [M+1] + ; 1 HNMR (300MHz, CDCl 3 , TMS): δ9.77 (d, 1H, J=6.6Hz), 8.99 (d, 1H, J=3.0Hz), 8.49 (d, 1H, J=7.5Hz), 7.67 (d, 1H, J= 9.0Hz), 7.57 (dd, 1H, J=7.4, 4.8Hz), 7.27 (t, 1H, J=7.4Hz), 7.11 (t, 1H, J=6.6Hz), 2.70 (s, 3H).
[0028] NP2-B: 15% yield; m.p.=238°C; ESI: 263.3 (100%) [M+1] + ; 1 HNMR (300MHz, CDCl 3 , TMS): δ9.64 (d, 1H, J=6.6Hz), 8.94 (d, 1H, J=2.6Hz), 8.58 (d, 1H, J=7.5Hz), 7.69 (d, 1H, J= 9.0Hz), 7.63 (dd, 1H, J=7.4, 4.8Hz), 7.26 (t, 1H, J=7.4Hz), 7.10 (t, 1H, J=6.6Hz), 2.74 (s, 3H).
[0029] The structural formulas of NP2-A and NP2-B are as follows:
...
Embodiment 3
[0031] Example 3. Synthesis of Indenaza naphthoquinone derivatives NP3-A and NP3-B
[0032] The method is the same as in Example 1, except that pyridine is used instead of 3-fluoropyridine to obtain a pair of indolizine aza naphthoquinone derivative isomers NP3-A and NP3-B.
[0033] NP3-A: 31% yield; m.p.=226-227°C; ESI: 321.2 (100%) [M+1] + ; 1 H NMR (300MHz, CDCl 3 , TMS): δ9.92 (d, 1H, J=7.2Hz), 9.01 (d, 1H, J=3.9Hz), 8.54 (d, 1H, J=7.5Hz), 8.34 (d, 1H, J= 9.0Hz), 7.64 (dd, 1H, J=7.5, 4.5Hz), 7.49 (t, 1H, J=8.0Hz), 7.24 (t, 1H, J=6.9Hz), 4.52 (q, 2H, J= 7.1Hz), 1.51(t, 3H, J=7.1Hz).
[0034] NP3-B: 12% yield; m.p.=200-201°C; ESI: 321.2 (100%) [M+1] + ; 1 H NMR (300MHz, CDCl 3 , TMS): δ9.78 (d, 1H, J=6.9Hz), 8.99 (d, 1H, J=3.6Hz), 8.55 (d, 1H, J=7.8Hz), 8.38 (d, 1H, J= 9.0Hz), 7.65 (dd, 1H, J=7.8, 4.5Hz), 7.47 (ddd, 1H, J=8.7, 6.9, 0.9Hz), 7.20 (td, 1H, J=6.9, 1.2Hz), 4.50 ( q, 2H, J=7.2Hz), 1.52(t, 3H, J=7.2Hz).
[0035] The structural formulas of NP3-A and NP3-B ...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 