2,3,5,6-tetrachloroaniline

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Example 7 is repeated, 16.0×10-3 mol of HI being introduced in place of 6.2×10-3 mol. After a reaction time of 2 hours under these same conditions, the degree of conversion of the 2,3,5,6-tetrachloroaniline is 98.5%. 3,5-Dichloroaniline is obtained with a yield of 98.7%, relative to the 2,3,5,6-tetrachloroaniline converted. The degree of hydrodechlorination of the solvent is 0.1%. After a reaction time of 2 hours

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Example 7 is repeated, 16.0×10-3 mol of HI being introduced in place of 6.2×10-3 mol. After a reaction time of 2 hours under these same conditions, the degree of conversion of the 2,3,5,6-tetrachloroaniline is 98.5%. 3,5-Dichloroaniline is obtained with a yield of 98.7%, relative to the 2,3,5,6-tetrachloroaniline converted. The degree of hydrodechlorination of the solvent is 0.1%. After a reaction time of 2 hours

反応条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 200 parts of phenol, 197 parts of 2,3,5,6-tetrachloroaniline, 20 parts of platinum-on-charcoal catalyst (3.7% strength) and 15 parts of aqueous hydroiodic acid (57% strength) are dehalogenated with hydrogen in a tantalum autoclave (0.85 l) during the course of 3.5 hours, whilst stirring, under a maximum pressure of 50 bars and at 155° C. After cooling of the reaction vessel and after releasing the pressure, the reaction mixture is diluted with 500 parts by volume of water, made alkaline with concentrated sodium hydroxide solution, mixed with toluene and separated from the platinum-on-charcoal catalyst by filtration under suction. The organic phase obtained by layer separation is freed from the solvent by distillation. 99.3% strength, 3,5-dichloroaniline is obtained in a yield of 97%, with complete conversion of 2,3,5,6-tetrachloroaniline, by distillation over a simple distillation bridge. After cooling of the reaction vessel separated from the platinum-on-charcoal catalyst by filtration under suction The organic phase obtained by layer separation is freed from the solvent by distillation

反応条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 200 parts of phenol, 197 parts of 2,3,5,6-tetrachloroaniline, 20 parts of platinum-on-charcoal catalyst (3.7% strength) and 15 parts of aqueous hydroiodic acid (57% strength) are dehalogenated with hydrogen in a tantalum autoclave (0.85 l) during the course of 3.5 hours, whilst stirring, under a maximum pressure of 50 bars and at 155° C. After cooling of the reaction vessel and after releasing the pressure, the reaction mixture is diluted with 500 parts by volume of water, made alkaline with concentrated sodium hydroxide solution, mixed with toluene and separated from the platinum-on-charcoal catalyst by filtration under suction. The organic phase obtained by layer separation is freed from the solvent by distillation. 99.3% strength, 3,5-dichloroaniline is obtained in a yield of 97%, with complete conversion of 2,3,5,6-tetrachloroaniline, by distillation over a simple distillation bridge. After cooling of the reaction vessel separated from the platinum-on-charcoal catalyst by filtration under suction The organic phase obtained by layer separation is freed from the solvent by distillation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 57.7 g (0.25 mol) of 2,3,5,6-tetrachloroaniline, 250 ml of 36% strength aqueous solution of hydrochloric acid, 5 ml of concentrated sulphuric acid and 5 g of a 5% strength palladium/active charcoal catalyst are introduced into an 0.7 l autoclave made of tantalum. The autoclave is flushed first with nitrogen and then with hydrogen. The dechlorination is carried out over the course of 2 hours at 250° C and a hydrogen pressure of 200 atmospheres gauge. After the reaction, the catalyst is filtered off and washed twice with hot water. The reaction solution together with the wash water is rendered alkaline and warmed. After cooling, the reaction product is extracted twice with 150 ml of methylene chloride. After distilling off the methylene chloride, and subsequent fractional distillation, 36 g of 3,5-dichloroaniline (yield: 89% of theory) are obtained. The autoclave is flushed first with nitrogen is carried out over the course of 2 hours at 250° C After the reaction the catalyst is filtered off washed twice with hot water warmed After cooling the reaction product is extracted twice with 150 ml of methylene chloride After distilling off

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2 g of 1,2,3,4-Tetrafluoroanthraquinone and 30 g of 2,3,5,6-tetrachloroaniline were charged in a 50 cc, four necked flask and then the reaction was carried out at 210° C. for about 10 hours. After completion of reaction, 2,3,5,6-tetrachloroaniline was distilled out from the reaction solution and a column purification thereof using a column with a silica gel was effected to give rise to 0.62 g of 2-(2,3,5,6-tetrachloroanilino)-1,3,4-trifluoroanthraquinone (Dye 11') (yield 17.8 mol %) and 0.53 g of 2,3-bis(2,3,5,6-tetrachloroanilino)-1,4-difluoroanthraquinone (Dye 27') (yield 10.6 mol %). The physical properties of Dye 11' and analytical values defining the compound are tabulated in Table 22 and the physical properties of Dye 27' and analytical values defining the compound are tabulated in Table 23. was distilled out from the reaction solution a column purification