反应详情

温度

135 °C

To a mixture of 3-[4-(4-chloro-2-cyano-1-pyrrolyl)benzyl]-2-ethylthio-7-methyl-3H-imidazo[4,5-b]pyridine (846 mg) in 1,3-dimethyl-2-imidazolidinone (10 ml) was added sodium azide (539 mg) and triethylamine hydrochloride (1.425 g) and stirred at 135° C. for 24 hours. The reaction mixture was poured into ice-water and the pH value was adjusted to 4 with 7% hydrochloric acid, extracted with ethyl acetate (twice) and the organic layer was washed with water, dried over magnesium sulfate and evaporated. The residue was crystallized from methyl cyanide and washed hot methyl cyanide to give 3-[4-[4-chloro-2-(1H-tetrazol-5-yl)-1-pyrrolyl]-benzyl]-2-ethylthio-7-methyl-3H-imidazo[4,5-b]pyridine(766 mg) as a brown solid. mp: 88°-90° C.

1. extractionextracted with ethyl acetate (twice) and the organic layer
2. washwas washed with water
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customThe residue was crystallized from methyl cyanide
6. washwashed hot methyl cyanide