反应详情

The above procedure of Example G-1 first procedes through the acid azide as seen by the following isolation of the acid azide as its monohydrochloride: To a solution chilled in an ice bath and containing 3.0 g. of 2,3-dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid hydrazide and 60 ml. of 6 N hydrochloric acid was added dropwise with stirring a solution containing 3.0 g. of sodium nitrite in 10 ml. of water over a 30 minute period. The reaction mixture was then stirred for an additional 1 hour, allowing the reaction mixture to warm up to room temperature. The separated solid was collected, washed with water and dried in a vacuum oven over P2O5 at 25° C. for 48 hours to yield 3.0 g. of 2,3-dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid azide monohydrochloride, m.p. >300° C.

1. temperatureTo a solution chilled in an ice bath
2. additioncontaining 3.0 g
3. additioncontaining 3.0 g
4. stirringThe reaction mixture was then stirred for an additional 1 hour
5. customThe separated solid was collected
6. washwashed with water
7. dry with materialdried in a vacuum oven over P2O5 at 25° C. for 48 hours
8. customto yield 3.0 g