反应详情

61 mg (0.47 mmol) of rac-2,4-dimethylpentane-1,2-diamine were added to 150 mg (0.43 mmol) of 6-chloro-8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-3-carboxylic acid Example 16A, 143 mg (0.45 mmol) of TBTU and 0.19 ml (1.70 mmol) of 4-methylmorpholine in DMF (1.5 ml), and the reaction mixture was stirred at RT overnight. The mixture was diluted with water/TFA and purified by prep. 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 three times with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered off and concentrated. This gave 162 mg (79% of theory, purity 96%) of the target compound.

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