反应详情

A mixture of tert-butyl 2-(dimethylamino)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamate (1.8 g, 6.49 mmol) in dichloromethane (15 ml) and hydrochloric acid (5N in diethyl ether, 50 ml, 250 mmol) is stirred for 18 hours at room temperature. The solvent is evaporated and the residue dissolved in water (100 ml), made basic with 32% aqueous sodium hydroxide and extracted twice with ethyl acetate. The combined organic layers are washed with water, dried with magnesium sulfate and the solvent is evaporated under reduced pressure affording N2,N2-dimethyl-[1,2,4]triazolo[1,5-a]pyridine-2,7-diamine (727 mg, 63.2%) as a yellow solid. Mp.: 236-8° C. MS: m/z=178.1 (M+H+).

1. customThe solvent is evaporated
2. dissolutionthe residue dissolved in water (100 ml)
3. extractionextracted twice with ethyl acetate
4. washThe combined organic layers are washed with water
5. dry with materialdried with magnesium sulfate
6. customthe solvent is evaporated under reduced pressure