反应详情

To a solution containing 2-(2-oxo-4-prop-2-ynyl-piperazin-1-ylmethyl)-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester (1.3 g, 3.53 mmol) in CH2Cl2 (100 mL) is added TFA (20 mL) at 0° C. After 6 h, the reaction mixture is concentrated to dryness and then partitioned between aqueous NaHCO3 (500 mL) and CH2Cl2 (200 mL) and the layers are separated. The aqueous phase is extracted four times with CH2Cl2 (100 mL) and the combined organic phase is washed with brine, dried over anhydrous Na2SO4, filtered and concentrated. The crude residue is purified by flash silica gel chromatography (CH2Cl2 to 10% MeOH/CH2Cl2) to provide 616 mg (65%) of the title compound as a pale yellow solid.

1. concentrationthe reaction mixture is concentrated to dryness
2. custompartitioned between aqueous NaHCO3 (500 mL) and CH2Cl2 (200 mL)
3. customthe layers are separated
4. extractionThe aqueous phase is extracted four times with CH2Cl2 (100 mL)
5. washthe combined organic phase is washed with brine
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude residue is purified by flash silica gel chromatography (CH2Cl2 to 10% MeOH/CH2Cl2)