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methyl 4-((3,5-dichloro-2-hydroxybenzyl)amino)-2-hydroxybenzoate[ No CAS ]
C36H32Cl2N4O7[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
triphosgene (150mg, 0.5mmol)Dissolve in 10 mL of dichloromethane under anhydrous anaerobic conditions.Cool to minus 78 °C,Add 10 mL of mixed solvent of pyridine and dichloromethane with stirring(pyridine: dichloromethane volume ratio = 1:9),The solution gradually appeared pale yellow from colorless and transparent, and a pale yellow precipitate gradually formed. After stirring for 15 minutes,Methyl 2-hydroxy-4-(2-hydroxy-3,5-dichlorobenzyl)aminobenzoate (methyl ester of ZL006, Synthetic method: Bioorganic & Medicinal Chemistry Letters, 2016, 26:2152-2155, 342mg, 1mmol)Dissolved in 10 mL of dichloromethane and added to the reaction flask over 30 minutes.Continue to be below zero when you are finished addingStir at 78°C for 30 minutes,Then it was raised to room temperature and reacted for 8 hours. 8 hours later, <strong>[1252003-15-8]Tubastatin A</strong> (671 mg, 2 mmol)Diluted with 10 mL of methylene chloride and added to the systemTriethylamine (400 mg, 6 mmol) was added. After the reaction was continued at room temperature for 24 hours, the sand was spun off and the product 001 was obtained by column chromatography