Application of triptolide amide derivatives in the preparation of drugs for the treatment of autoimmune diseases
A technology of tripterygium amide and immune diseases, which is applied in the fields of medicinal chemistry and pharmacotherapeutics, can solve the problems of toxicity, narrow safe treatment range, and limited clinical application, etc., achieves small toxic and side effects, significant curative effect, and relieves rheumatoid The effect of arthritis
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Embodiment 1
[0024]
[0025] Triptolide 22mg (0.048mmol) was dissolved in 1mL of anhydrous DMF, followed by adding PyBop (50mg, 0.096mmol), N,N-diisopropylethylamine (20μL, 0.12mmol), methylamine hydrochloride ( 0.05 mmol), and reacted at room temperature for 24 hours. Add 15 ml of deionized water, extract three times with ethyl acetate, combine the organic phases, dry with anhydrous magnesium sulfate, filter and spin dry to obtain the crude product. Column chromatography (dichloromethane / methanol) gave a red solid (compound I) in 61% yield.
[0026] 1 H NMR (600MHz, CDCl 3 )δ H 7.00(1H,d,J=8.0Hz,H-6),6.99(1H,s),6.51(1H,s,H-1),6.32(1H,d,J=8.0Hz,H-7), 5.80(1H,s,NH), 2.66(3H,s,NHCH3), 2.19(3H,s,H-23), 1.42(3H,s,H-25), 1.24(3H,s,H-26) ,1.14(3H,s,H-30),1.11(3H,s,H-28),0.60(3H,s,H-27); 13 C NMR (100MHz, CDCl 3 )δ C 178.5(C-2), 178.3(C-29), 170.4(C-8), 164.8(C-10), 146.0(C-3), 134.1(C-6), 127.4(C-5), 119.5 (C-1), 118.0(C-7), 117.1(C-4), 45.1(C-14), 44.4(C-18), 43.0(C-9), 40.3(C-20)...
Embodiment 2
[0028]
[0029] Triptolide 22mg (0.048mmol) was dissolved in 1mL of anhydrous DMF, followed by adding PyBop (50mg, 0.096mmol), N,N-diisopropylethylamine (20μL, 0.12mmol), ethylamine hydrochloride ( 0.05 mmol), and reacted at room temperature for 24 hours. Add 15 ml of deionized water, extract three times with ethyl acetate, combine the organic phases, dry with anhydrous magnesium sulfate, filter and spin dry to obtain the crude product. Column chromatography (dichloromethane / methanol) gave a red solid (compound II) in 54% yield.
[0030] 1 H NMR (400MHz, CDCl 3 )δ H 7.02(1H,d,J=8.0Hz,H-6),7.01(1H,s),6.53(1H,s),6.34(1H,d,J=8.0Hz,H-7),5.69(1H, s,NH), 3.16(2H,m,H-1'), 2.21(3H,s,H-23), 1.43(3H,s,H-25), 1.26(3H,s,H-26), 1.15(3H,s,H-30), 1.12(3H,s,H-28), 0.65(3H,s,H-27); 13 C NMR (100MHz, CDCl 3 )δ C178.1(C-2), 177.5(C-29), 170.5(C-8), 164.8(C-10), 145.9(C-3), 134.2(C-6), 127.2(C-5), 119.3 (C-1), 117.9(C-7), 117.0(C-4), 44.9(C-14), 44.2(C-18), 42.9(C-9), 40.0(C-20), 39....
Embodiment 3
[0032] In vitro cell activity studies of triptolide amide derivatives
[0033] experiment material
[0034] CCK-8 cell viability assay kit was purchased from Dojindo Laboratories. Fetal bovine serum and RPMI 1640 medium were purchased from Invitrogen. Methotrexate was purchased from Shanghai Oriental Pharmaceutical Technology Experiment Co., Ltd. Red blood cell lysate was purchased from Jiangsu Kaiji Biotechnology Co., Ltd. Concanavalin A (ConA) was purchased from Sigma. Male BALB / c mice (6-8 weeks old, 18-25 g) were purchased from the Model Animal Center of Nanjing University.
[0035] experiment method
[0036] The Balbc mice were sacrificed by dissecting their cervical vertebrae, immersed in 75% alcohol for 3 minutes, and the spleen was isolated. The spleen was ground and passed through a 200-mesh sterile filter. After removal of cell debris and clumps, single cell suspensions were prepared. Red blood cells are lysed in red blood cell lysis buffer. Then, the cell p...
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