Antibody Drug Conjugates with Two Different Drugs
A technology of drug conjugates and antibodies, which is used in drug combinations, medical preparations with non-active ingredients, and medical preparations containing active ingredients, etc. It is difficult to determine the coupling position, and the selectivity of amino coupling is poor.
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Embodiment 1-6
[0076]
Embodiment 1
[0077] Example 1 Synthesis of Compound 1
[0078]
[0079] Fmoc-Lys(mmt)-OH (2g, 3.2mmol, 1eq), PABA (788.16mg, 6.4mmol, 2eq), HATU (1.34g, 3.52mmol, 1.1eq), DIEA (1.24g, 9.6 mmol, 3eq) and 20ml DMF, stir and dissolve, nitrogen protection, reaction at 25°C; dot plate detection, lysine reaction is complete. 200ml of water was added to the reaction solution, a large amount of solid was precipitated, extracted with EA (60ml×3), the organic phase was washed three times with brine, dried over anhydrous sodium sulfate, and spin-dried to obtain 2.85g of yellow oil. The intermediate of the previous step was dissolved with 20 ml of diethylamine, and the reaction was carried out at 25°C under nitrogen protection; The solvent was spin-dried, 100 ml of EA was added to dissolve, washed with brine three times, dried over anhydrous sodium sulfate, and spin-dried to obtain 2.58 g of a light brown oily product. Purification by column chromatography: gradient elution was carried out with D...
Embodiment 2
[0081] Example 2 Synthesis of Compound 2
[0082]
[0083] Compound 1 (300 mg, 0.574 mmol, 1 eq) N was added to a single-necked flask 3 PEG 8 COOH (350mg, 0.631mmol, 1.1eq), HOBT (85mg, 0.631mmol, 1.1eq) DIEA (149mg, 1.15mmol, 2.0eq) and 4ml of dry DMF, nitrogen protection, ice water bath cooling and stirring to dissolve the solution; add HATU (240mg , 0.631mmol, 1.1eq), 25 ℃ reaction; spot plate detection, 005 reaction is complete, post-processing. 50 ml of water was added to the reaction solution, extracted with EA (50 ml×3), the organic phase was washed three times with brine, dried over anhydrous sodium sulfate, and spin-dried to obtain 920 mg of light yellow oil. Preparation and purification of thin layer plate: develop once with DCM:MeOH=15:1 as developing solvent, and purify to obtain 500 mg of light yellow oily product.
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