Antibody-drug-conjugate, and intermediate, preparation method and application thereof
An antibody-conjugated drug and antibody technology, applied in the field of biotechnology and medicine, can solve the problem of single type of antibody-conjugated drug
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preparation example 1
[0103] Preparation Example 1 Preparation of DS-8201a linker-drug conjugate GGFG-Dxd
[0104] The compound GGFG-Dxd (structure as follows) was synthesized according to the known method reported in WO2015146132A1, ESI-MS m / z: 1034.5 (M+H), 1 H-NMR (400MHz, DMSO-d 6 )δ8.61(t, J=6.4Hz, 1H), 8.50(d, J=8.5Hz, 1H), 8.28(t, J=5.1Hz, 1H), 8.11(d, J=7.5Hz, 1H) ,8.05(t,J=5.7Hz,1H),7.99(t,J=5.9Hz,1H),7.77(d,J=11.0Hz,1H),7.31(s,1H),7.25–7.16(m, 5H), 6.98(s, 2H), 6.51(s, 1H), 5.59(dt, J=7.4, 4.1Hz, 1H), 5.41(s, 2H), 5.20(s, 2H), 4.64(d, J =6.1Hz,2H),4.53–4.40(m,1H),4.02(s,2H),3.74–3.37(m,8H),3.18–3.00(m,2H),3.04–2.97(m,1H), 2.77(dd,J=13.5,9.4Hz,1H),2.38(s,3H),2.19(dd,J=14.9,8.5Hz,2H),2.11–2.05(m,2H),1.86(dd,J= 14.0,6.7Hz,2H),1.45(s,4H),1.20–1.14(m,2H),0.87(t,J=7.1Hz,3H).
[0105]
Embodiment 1
[0106] The synthesis of embodiment 1 compound DX01
[0107]
[0108] Synthesis of step 1 compound IIIC:
[0109] Commercially available compound IIIA (5.58g, 10mmol) and commercially available IIIB (3.16g, 10mmol) were mixed in 100mL of anhydrous N, N-dimethylformamide, HATU (1.14g, 3.0mmol) was added, three Ethylamine 10mL, react at room temperature for 2h. After the reaction was complete, the solvent was distilled off under reduced pressure, and the crude product was purified by silica gel column chromatography [chloroform:methanol=10:1 (v / v)] to obtain the title compound IIIC (7.71g, yield 90%), ESI-MS m / z : 857.1 (M+H).
[0110] Synthesis of step 2 compound IIID:
[0111] Compound IIIC (7.71 g, 9 mmol) was dissolved in dichloromethane, 9 mL of trifluoroacetic acid was added, and reacted at room temperature for 0.5 h. After the reaction was completed, the solvent was distilled off under reduced pressure, and the crude product was purified by silica gel column chromat...
Embodiment 2
[0121] Synthesis of DX02, DX03, DX04
[0122]
[0123] Referring to Example 1, in step 1, compound IIIA was reacted with different commercially available amino fragments, and the subsequent steps were the same as in Example 1 to finally obtain compounds DX02-DX04.
[0124] Compound DX02: light yellow powder, ESI-MS m / z: 1164.3 (M+H); Compound DX03: light yellow powder, ESI-MS m / z: 1199.5 (M+H); Compound DX04: light yellow powder, ESI - MS m / z: 1169.2 (M+H).
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