反应详情

77 mg (0.66 mmol) of rac-2-methylpentane-1,2-diamine were added to 200 mg (0.60 mmol) of 8-[(2,6-difluorobenzyl)oxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid Example 21A, 203 mg (0.63 mmol) of TBTU and 0.27 ml (2.41 mmol) of 4-methylmorpholine in DMF (2.1 ml), and the reaction mixture was stirred at RT overnight. The mixture was diluted with water/TFA and purified by preparative RP-HPLC (acetonitrile/water gradient with addition of 0.1% TFA). The product fraction was concentrated. Saturated aqueous sodium bicarbonate solution was added to the residue, and the mixture was extracted twice with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered off and concentrated. This gave 199 mg (76% of theory, purity 99%) of the target compound.

1. custompurified by preparative RP-HPLC (acetonitrile/water gradient with addition of 0.1% TFA)
2. concentrationThe product fraction was concentrated
3. additionSaturated aqueous sodium bicarbonate solution was added to the residue
4. extractionthe mixture was extracted twice with dichloromethane
5. dry with materialThe combined organic phases were dried over sodium sulphate
6. filtrationfiltered off
7. concentrationconcentrated