反应详情

70 mg (0.60 mmol) of 2-ethylbutane-1,2-diamine were added to 100 mg (0.30 mmol) of 8-[(2,6-difluorobenzyl)oxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid Example 21A, 145 mg (0.45 mmol) of TBTU and 0.13 ml (1.20 mmol) of 4-methylmorpholine in DMF (1.9 ml), and the reaction mixture was stirred at RT overnight. The mixture was then diluted with water/TFA and purified by preparative RP-HPLC (acetonitrile/water gradient with addition of 0.1% TFA). After concentration, the residue was taken up in dichloromethane and washed twice with saturated aqueous sodium bicarbonate solution. The aqueous phase was extracted twice with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered off, concentrated and lyophilized. This gave 110 mg (85% of theory, purity 100%) of the target compound.

1. custompurified by preparative RP-HPLC (acetonitrile/water gradient with addition of 0.1% TFA)
2. concentrationAfter concentration
3. washwashed twice with saturated aqueous sodium bicarbonate solution
4. extractionThe aqueous phase was extracted twice with dichloromethane
5. dry with materialThe combined organic phases were dried over sodium sulphate
6. filtrationfiltered off
7. concentrationconcentrated