反应详情

温度

55 °C

1450 parts K3Fe(CN)6, 595 parts Na2CO3, and 4150 parts water were added to a 12-liter round bottom flask equipped with a mechanical stirrer, thermometer, and addition funnel. The mixture was heated to 55° C. with stirring. A solution of 227 parts 4-(N,N-diethylamino)-2-methylaniline monohydrochloride, 128 parts o-chlorophenol, 1960 parts ethanol, and 2500 parts water was charged to the addition funnel and added dropwise to the stirred, heated solution. After the addition was complete the reaction mixture was maintained at 55° C. with stirring for 20 minutes. The warm mixture was filtered with vacuum and the resulting filter cake was placed in a solution of 296 parts ethanol and 1125 parts water to form a slurry. The dye was isolated by vacuum filtration. This process was repeated two times, first with 296 parts ethanol and 1125 parts water, then with 608 parts methanol. After the final vacuum filtration the filter cake was dried at 40° C. under vacuum for 48 hours. Yield was ~90%. The final product can be recrystallized from ethyl acetate or ethanol.

1. customequipped with a mechanical stirrer
2. additionthermometer, and addition funnel
3. additionadded dropwise to the stirred
4. temperatureheated solution
5. additionAfter the addition
6. temperaturewas maintained at 55° C.
7. stirringwith stirring for 20 minutes
8. filtrationThe warm mixture was filtered with vacuum
9. filtrationthe resulting filter cake
10. customto form a slurry
11. customThe dye was isolated by vacuum filtration
12. filtrationAfter the final vacuum filtration the filter cake
13. customwas dried at 40° C. under vacuum for 48 hours
14. customThe final product can be recrystallized from ethyl acetate or ethanol