反应详情

2-Hydrazino-quinazolin-4-one (IIIb) (17.6 g; 0.1 mole), was suspended in 2 N-hydrochloric acid (78 ml; 0.156 mole) in a 600 ml beaker equipped with a thermometer and efficient stirrer. 15% w/v aqueous NaNO2 solution was added at such a rate that the temperature remained between 20° and 25° C., cooling with a water bath when necessary, until a small permanent excess of nitrous acid was present. The volume of the nitrite solution used was 63 ml (=9.45 g NaNO2 ; 0.137 mole). The reaction mixture was then stirred for 1 hour, filtered, and the solid washed acid free with water. After pulling as dry as possible on the filter, the product was dried completely in a vacuum desiccator over phosphorus pentoxide.

1. custombeaker equipped with a thermometer and efficient stirrer
2. additionwas added at such a rate that the temperature
3. customremained between 20° and 25° C.
4. temperaturecooling with a water bath when necessary
5. filtrationfiltered
6. washthe solid washed acid free with water
7. customas dry as possible on the filter
8. dry with materialthe product was dried completely in a vacuum desiccator over phosphorus pentoxide