反应详情

A mixture of 78.0 mg (0.235 mmol, 1.0 eq.) of 7-[(2,6-difluorobenzyl)oxy]-2,5-dimethylpyrazolo[1,5-a]pyridine-3-carboxylic acid from Example 4A, 49 μl (0.47 mmol, 2.0 eq.) of 1,2-diamino-2-methylpropane [CAS No.: 811-93-8] and 0.20 ml (1.2 mmol, 5.0 eq.) of N,N-diisopropylethylamine in 2.4 ml of DMF was admixed with 116 mg of HATU (0.305 mmol, 1.3 eq.) and stirred at RT for 6 h. Subsequently, water was added and the mixture was extracted three times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate, filtered and concentrated. The residue was stirred with water, and the precipitated solids were filtered off and purified by means of preparative HPLC (Method 4). 22.3 mg of the title compound were obtained (24% of theory).

1. extractionthe mixture was extracted three times with ethyl acetate
2. washThe combined organic phases were washed with saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated
6. stirringThe residue was stirred with water
7. filtrationthe precipitated solids were filtered off
8. custompurified by means of preparative HPLC (Method 4)