反应详情

A mixture of 0.9 g (2.0 mmol) 2-(3,4-dimethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-butanoic acid, 0.71 g (2.2 mmol) TBTU, 0.28 g (2.1 mmol) HOBt, 0.39 mL (2.2 mmol) ethyldiisopropylamine, 45 mL THF and 5 mL water was stirred for 10 min at RT, combined with 0.37 g (2.1 mmol) [1,4′]bipiperidinyl and stirred for a further 4 h. The reaction mixture was evaporated down under reduced pressure, the residue was combined with saturated NaHCO3 solution and extracted three times with DCM/MeOH (95:5). The combined organic phases were dried, evaporated down under reduced pressure and purified by chromatography over silica gel. The product fractions were evaporated down under reduced pressure, the residue was triturated with diisopropylether and suction filtered.

1. stirringstirred for a further 4 h
2. customThe reaction mixture was evaporated down under reduced pressure
3. extractionextracted three times with DCM/MeOH (95:5)
4. customThe combined organic phases were dried
5. customevaporated down under reduced pressure
6. custompurified by chromatography over silica gel
7. customThe product fractions were evaporated down under reduced pressure
8. customthe residue was triturated with diisopropylether and suction
9. filtrationfiltered