Method for preparing novel Bc1-2 protein inhibitor derived from ABT-263
A technology of organic solvents and compounds, applied in the field of synthesis of novel Bcl-2 protein inhibitors
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Embodiment 1
[0049] Synthesis of Compound 2-1
[0050] In a 1L three-necked flask equipped with mechanical stirring, 37 g (149.6 mmol) of (R)-N-tert-butoxycarbonylaspartic acid-4-methyl ester was dissolved in 400 mL THF, and cooled to -10°C. 15.1g (149.6mmol) N-methylmorpholine was added dropwise with stirring, and after the dropwise addition, 16.2g (179.6mmol) ethyl chloroformate was slowly added, and the temperature was controlled at -10°C-5°C. React for 1 hour, add 17g (448mmol) sodium borohydride at one time, add 100mL methanol dropwise at 0°C, stir for 1 hour, add 400mL water, extract with ethyl acetate (4*200mL), combine organic phases, dry and concentrate , 31 g of the product was obtained after column chromatography, and the yield was 86%.
[0051] Synthesis of compound 2-2
[0052] In a three-necked flask equipped with magnetic stirring, 32.5 g (186.5 mmol) of diethyl azodicarboxylate and 48.9 g (186.5 mmol) of triphenylphosphine were dissolved in 500 mL of anhydrous dichloromet...
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