反应详情

A solution of 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether, (8.0 g, 0.028 mole), p-chloroglycolanilide (5.23 g, 0.028 mole), 170 ml of tetrahydro-furan, 120 ml of n-hexane, and 4.5 ml of glacial acetic acid was refluxed for about 8.5 hours, replacing solvent as distillate was removed. Color was then discharged by the addition of 20 drops of tetramethylguanidine and the solution was filtered hot. Hexane was added to the filtrate, yielding a light green oil. The oil was removed and the hexane solution, on cooling, gave a light blue solid. The solid was filtered, washed with petroleum ether and dried. Recrystallization from 150 ml methylcyclohexane/40 ml acetone gave a yellow-white, gummy solid. This was recrystallized from VM&P naphtha to give a fine white powder, mp 137.5°-140° C.

1. customwas removed
2. additionColor was then discharged by the addition of 20 drops of tetramethylguanidine
3. filtrationthe solution was filtered hot
4. additionHexane was added to the filtrate
5. customyielding a light green oil
6. customThe oil was removed
7. temperaturethe hexane solution, on cooling
8. customgave a light blue solid
9. filtrationThe solid was filtered
10. washwashed with petroleum ether
11. customdried
12. customRecrystallization from 150 ml methylcyclohexane/40 ml acetone
13. customgave a yellow-white, gummy solid
14. customThis was recrystallized from VM&P naphtha
15. customto give a fine white powder, mp 137.5°-140° C.