Reacción #709504

Ecuación de reacción

5-nitro-1,4,4a,9a-tetrahydroanthraquinone

toluene

sodium bisulfide

→

1-aminoanthraquinone

Rendimiento 99.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroA 2 liter autoclave equipped with anchor stirrer
2. 2
   workup.STIRRINGStirring
3. 3
   Otrothe lower layer is separated under this pressure
4. 4
   TemperaturaThe upper phase is cooled to room temperature, whereupon the pure 1-aminoanthraquinone
5. 5
   Otrocrystallises
6. 6
   Otrois then isolated by filtration
7. 7
   Lavadowashed with 75 parts of toluene and vaccum
8. 8
   Otrodried at 80° C
9. 9
   workup.ADDITIONIn the further batches, the bulk (e.g. 3/4) of the toluene-containing mother liquor

Procedimiento

A 2 liter autoclave equipped with anchor stirrer is charged with 64.3 parts of 5-nitro-1,4,4a,9a-tetrahydroanthraquinone, 750 parts of toluene, 250 parts of water and 8.8 parts of sodium bisulfide. With stirring, the phase mixture is heated to 160° C. under an excess pressure of 10 to 11 bar. Stirring is then discontinued and the lower layer is separated under this pressure. The upper phase is cooled to room temperature, whereupon the pure 1-aminoanthraquinone crystallises and is then isolated by filtration, washed with 75 parts of toluene and vaccum dried at 80° C. In the further batches, the bulk (e.g. 3/4) of the toluene-containing mother liquor is used instead of fresh toluene. In this manner 55 parts of 1-aminoanthraquinone in 99% purity are obtained, corresponding to a yield of about 99% of theory.

Fuente