反应详情

8.0 grams (0.0275 mole) of the acid chloride of the product of Example 2 was reacted with excess dimethylamine in 200 mls of toluene. This solution was heated on a steam bath for 2 hours. The solution was filtered and the filtrate distilled at reduced pressure. The residual solid was filtered, washed with petroleum ether and air dried. There was isolated 5.0 grams of a solid which when recrystallized from absolute ethyl alcohol gave 2.5 grams of a white solid that melted at 278° C. The infrared spectrum showed two carbonyl bands one at 6.0μ, the other a 6.1μ. Analysis calculated for C19H17N3O2.1H2O, C, 70.4; H, 5.4; N, 12.9. Found: C, 70.1; H, 5.5; N, 12.9.

1. temperatureThis solution was heated on a steam bath for 2 hours
2. filtrationThe solution was filtered
3. distillationthe filtrate distilled at reduced pressure
4. filtrationThe residual solid was filtered
5. washwashed with petroleum ether and air
6. customdried