Reductive alkylation method for glycopeptide antibiotics
A technology of glycopeptide antibiotics and alkylation, which is applied in the preparation method of peptides, chemical instruments and methods, peptides, etc., can solve the problems of low yield and many secondary substitution impurities, achieve high yield and control by-products Effect
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Embodiment 1
[0028] Add A82846B (0.446g, 0.28mmol) to 45ml of anhydrous methanol, stir at room temperature for 0.5h, add DIEA (550ul, 3.3mmol, 11.9eq), stir at room temperature for 0.5h, add copper acetate monohydrate (56mg, 0.28mmol , 1eq) continued to stir for 2h, added 4'-chloro-4-biphenylcarbaldehyde (212.3mg, 0.98mmol, 3.5eq), and continued to stir for 24h. Under the protection of nitrogen, the system was cooled to 0-10°C, trifluoroacetic acid (278.9ul, 3.64mmol, 13eq) was added, and after the reaction was stirred for 1h under temperature control, TBAB (40mg, 0.46mmol, 1.6eq) was added to the reaction in 4 times solution (0.4eq / time / hour), add and react for 1h. The reaction solution was taken for HPLC detection. After the reaction is finished, add 1mol / L sodium hydroxide solution dropwise to adjust the pH of the system to 9.0, concentrate under reduced pressure to leave about 15ml, add 15ml of acetonitrile dropwise into the system, stir and crystallize for 1 hour, filter with suction...
Embodiment 2
[0031] Add A82846B (0.43g, 0.27mmol) to 43ml of anhydrous methanol, stir at room temperature for 0.5h, add DIEA (267ul, 1.62mmol, 6eq), stir at room temperature for 0.5h, add copper acetate monohydrate (53.9mg, 0.27mmol , 1eq) continued to stir for 2h, added 4'-chloro-4-biphenylcarbaldehyde (204.75mg, 0.945mmol, 3.5eq), and continued to stir for 24h. Under the protection of nitrogen, the system was cooled to 0-10°C, trifluoroacetic acid (206.9ul, 2.7mmol, 10eq) was added, and after stirring for 1 hour under temperature control, TBAB (37.57mg, 0.432mmol, 1.6eq) was added to the In the reaction solution (0.4eq / time / hour), the reaction was completed for 1h. The reaction solution was taken for HPLC detection. After the reaction is finished, add 1mol / L sodium hydroxide solution dropwise to adjust the pH of the system to 9.0, concentrate under reduced pressure to leave about 15ml, add 15ml of acetonitrile dropwise into the system, stir and crystallize for 1 hour, filter with suctio...
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