Compounds based on crbn ligand-induced degradation of parp-1 and preparation methods and applications
A PARP-1, compound technology, applied in the field of pharmaceutical compound synthesis, can solve problems such as side effects
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Embodiment 1
[0049] (1) Preparation of 8-amino-N-(2-(2,6-dioxopiperidin-3-yl)-1-oxoisoisoin-4-yl)octamide (2-1):
[0050]
[0051] Add lenalidomide (10mmol) and 8-((tert-butoxycarbonyl)amino)octanoic acid (10mmol) into a 50mL round bottom flask, add 10mL of anhydrous DMF (N,N-dimethylformamide) to dissolve, Then HATU (10.5mmol, 2-(7-benzotriazole oxide)-N,N,N',N'-tetramethyluronium hexafluorophosphate) and TEA (10.5mmol, triethylamine) were added, The reaction was carried out at room temperature 25° C. for 12 hours under the protection of nitrogen. After the reaction is complete, pour the reaction solution into water, extract with ethyl acetate, combine the organic phases, wash with saturated brine, dry over anhydrous sodium sulfate, and distill under reduced pressure to obtain an unpurified white crude product; take 1.0 mmol of the above crude product and add 3 mL of TFA (Trifluoroacetic acid) and DCM (dichloromethane) mixed solvent TFA / DCM (1:5, v / v), reacted at room temperature 25 °...
Embodiment 2
[0057] Preparation of N-(11-((2-(2,6-dioxopiperidin-3-yl)-1-oxoisoisoin-4-yl)amino)-11-oxoisopentenyl)- 2-Fluoro-5-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzamide (1-2). Referring to Example 1 for the specific preparation method, it is only necessary to replace the 8-((tert-butoxycarbonyl)amino)octanoic acid in Example 1 with 11-((tert-butoxycarbonyl)amino)undecanoic acid. 1-2 Its structure is as follows:
[0058]
[0059] The characterization results are as follows: 1 H NMR(500MHz,DMSO-d6)δ12.62(s,1H),11.05(s,1H),9.78(s,1H),8.28(d,J=7.8Hz,1H),8.25(s,1H) ,7.97(d,J=7.9Hz,1H),7.89(t,J=8.3Hz,1H),7.83(t,J=8.2Hz,2H),7.55(d,J=6.8Hz,1H),7.51 (d,J=5.3Hz,1H),7.47–7.42(m,1H),7.23–7.17(m,1H),5.18(dd,J=13.3,5.1Hz,1H),4.33(s,2H), 3.40(s,3H),3.22(dd,J=13.0,6.7Hz,2H),2.99–2.90(m,1H),2.63(d,J=17.0Hz,1H),2.36(d,J=7.6Hz ,2H),2.00(s,1H),1.63–1.46(m,4H),1.28(d,J=15.4Hz,12H).13C NMR(126MHz,DMSO-d6)δ173.33,171.88,171.55,168.33,163.89 ,159.87,157.29,145.40,134.77,134.29,134.12,133.95,13...
Embodiment 3
[0061]Preparation of N-(12-((2-(2,6-dioxopiperidin-3-yl)-1-oxoisoisoin-4-yl)amino)-12-oxodecyl)-2- Fluoro-5-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzamide (1-3). Referring to Example 1 for the specific preparation method, it is only necessary to replace the 8-((tert-butoxycarbonyl)amino)octanoic acid in Example 1 with 12-((tert-butoxycarbonyl)amino)dodecanoic acid. Its structure is as follows:
[0062]
[0063] The characterization results are as follows: 1 H NMR (500MHz, DMSO-d6) δ12.61(s, 1H), 11.04(s, 1H), 9.77(s, 1H), 8.27(d, J=7.8Hz, 1H), 8.24(t, J= 4.7Hz, 1H), 7.97(d, J=7.9Hz, 1H), 7.88(t, J=7.6Hz, 1H), 7.86–7.78(m, 2H), 7.54(dd, J=6.8, 2.3Hz, 1H),7.51–7.50(m,1H),7.47–7.41(m,1H),7.25–7.14(m,1H),5.16(dd,J=13.3,5.1Hz,1H),4.33(s,2H) ,3.37(s,4H),3.20(dd,J=13.0,6.7Hz,2H),2.98–2.88(m,1H),2.62(d,J=16.9Hz,1H),2.37–2.34(m,2H ),1.63–1.45(m,4H),1.31–1.23(m,14H).13C NMR(126MHz,DMSO-d6)δ173.33,171.87,171.55,168.32,163.88,159.86,157.27,145.41,134.77,134.23,13 ,133.97,133...
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