反应详情

3.0 g (8.9 mmol)-8-(trans-2,3-dihydro-2-hydroxy-1-indenylamino)-2,3-dimethyl-imidazo[1,2-a]pyridine-6-carboxylic acid and 3.7 g (11.6 mmol) —O-(1H-benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TBTU) are suspended in 150 ml dichloromethane and 3.2 ml (17.8 mmol) dimethylamine (5.6 M in ethanol) are added to the reaction mixture. After stirring for 16 h at room temperature, the reaction mixture is extracted with saturated aqueous sodium hydrogencarbonate. The organic phase is separated, dried over anhydrous magnesium sulphate and evaporated. The residue is dissolved in 10 ml dichloromethane and 50 ml diethyl ether are added. After stirring for 30 min, the precipitate is collected, washed with diethyl ether and dried in vacuo to give 2.35 g (73%) of the title compound as a colourless solid (m.p. 148-149° C.).

1. extractionthe reaction mixture is extracted with saturated aqueous sodium hydrogencarbonate
2. customThe organic phase is separated
3. dry with materialdried over anhydrous magnesium sulphate
4. customevaporated
5. dissolutionThe residue is dissolved in 10 ml dichloromethane
6. addition50 ml diethyl ether are added
7. stirringAfter stirring for 30 min
8. customthe precipitate is collected
9. washwashed with diethyl ether
10. customdried in vacuo