Dichloromethane → Ammonia methanol dichloromethane

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Reaction Steps

A solution of (2-{5-[2-(6-methyl-pyridin-2-yl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-pyridin-3-ylcarbamoyl}-ethyl)-carbamic acid tert-butyl ester (Intermediate 59) (1 eq, 1.54 mmol, 774 mg) in DCM (100 ml) is cooled to 5° C. using an ice bath. Then TFA (20 eq, 32.7 mmol, 2.52 ml) is added within 5 min, the cooling bath is removed, and the mixture is stirred for 1 h at r.t. After addition of saturated aqueous K2CO3 solution the layers are separated and the aqueous layer is concentrated. The residue is taken up in MeCN, filtered, and the filtrate is concentrated. Column chromatography (DCM/MeOH/NH3) yields the title compound; [M+H]+=374;

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