反应详情

0.90 g (2.80 mmol) TBTU, 0.35 g (2.55 mol) HOBt, 0.49 mL (2.80 mmol) ethyldiisopropylamine was added to a mixture of 1.15 g (2.55 mol) 3-(3,4-dimethyl-phenyl)-2-{[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidine-1-carbonyl]-amino}-propionic acid and 100 mL THF and the mixture was stirred for 30 min at RT. Then 20 mL DMF was added, the mixture was stirred for 15 min and combined with 0.49 g (2.65 mmol) 1-methyl-4-piperidin-4-yl-piperazine. The reaction mixture was stirred overnight at RT, evaporated down under reduced pressure and the residue was combined with 70 mL saturated NaHCO3 solution. The aqueous phase was extracted three times with DCM, the combined organic phases were dried over Na2SO4, filtered and evaporated down under reduced pressure. The residue was purified by column chromatography over silica gel, the product fractions were evaporated down under reduced pressure, triturated with diethyl ether and suction filtered.

1. stirringthe mixture was stirred for 15 min
2. stirringThe reaction mixture was stirred overnight at RT
3. customevaporated down under reduced pressure
4. extractionThe aqueous phase was extracted three times with DCM
5. dry with materialthe combined organic phases were dried over Na2SO4
6. filtrationfiltered
7. customevaporated down under reduced pressure
8. customThe residue was purified by column chromatography over silica gel
9. customthe product fractions were evaporated down under reduced pressure
10. customtriturated with diethyl ether and suction
11. filtrationfiltered