反応 #1818188

反応方程式

hydrogen

sodium hydroxide

5-nitrotetrahydroanthraquinone

dipropylene glycol

→

1-aminoanthraquinone

収率 87.3%

反応条件

後処理

1. 1
   その他at 120° C.
2. 2
   その他Hydrogen was absorbed in the starting 5-nitro compound in an amount of 2mols per mol of the 5-nitro compound
3. 3
   ろ過After completion of the hydrogenation, the resultant solution was subjected to filtration under hot conditions at 120° to 130° C.
4. 4
   その他to remove the catalyst
5. 5
   workup.ADDITIONTo the resultant filtrate was added 350 grams of water for dilution
6. 6
   その他to obtain crystals which
7. 7
   その他were separated by filtration
8. 8
   洗浄washed with water
9. 9
   その他dried

実験手順

0.1 Gram of a 5% palladium on carbon catalyst and 10 grams of a 20% aqueous sodium hydroxide solution were added to a mixture of 12.8 grams of 5-nitrotetrahydroanthraquinone and 170 grams of dipropylene glycol in an autoclave, into which was fed hydrogen, until the pressure reached 25 kg/cm2, for hydrogenation of the 5-nitro compound at 120° C. with agitation. Hydrogen was absorbed in the starting 5-nitro compound in an amount of 2mols per mol of the 5-nitro compound. After completion of the hydrogenation, the resultant solution was subjected to filtration under hot conditions at 120° to 130° C. to remove the catalyst therefrom. To the resultant filtrate was added 350 grams of water for dilution to obtain crystals which were separated by filtration, washed with water and dried to yield 9.7 grams of 1-aminoanthraquinone having a purity of 96.7%.

出典