反应详情

To a mixture containing nitromethane (7.4 g., 0.12 moles), benzofuroxan (13.6 g., 0.10 moles) and tetrahydrofuran (50 ml.) is slowly added dimethylpyrimidine (11.3 g.) dropwise. The heat of reaction causes the reaction temperature to rise sharply; therefore, an ice-bath is used to maintain a steady rate of reflux. Upon completion of addition, the resulting mixture is allowed to cool to room temperature whereupon the solid product which precipitates is filtered, washed with water, dried and recrystallized from a MeOH/NaOCH3 mixture which is subsequently acidified. The crystalline product has an M.P. 213° C. dec.

1. temperatureThe heat of reaction
2. customtherefore, an ice-bath is used
3. temperatureto maintain a steady rate
4. temperatureof reflux
5. additionUpon completion of addition
6. customprecipitates
7. filtrationis filtered
8. washwashed with water
9. customdried
10. customrecrystallized from a MeOH/NaOCH3 mixture which