تفاعل #1797494

معادلة التفاعل

5-(N-acetylamino)indane

p-iodotoluene

potassium carbonate

potassium hydroxide

→

indan-5-yl-p-tolylamine

المذيبات

water

water

isoamyl alcohol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwhile introducing a nitrogen gas
2. 2
   أخرىhydrolysis at 130° C. for 2 hours
3. 3
   workup.ADDITIONwas added
4. 4
   أخرىIsoamyl alcohol was removed by azeotropic distillation
5. 5
   workup.ADDITION200 ml of toluene was added
6. 6
   workup.DISSOLUTIONto dissolve the reaction product
7. 7
   ترشيحAfter filtration
8. 8
   ترشيحAfter filtering out the magnesium sulfate
9. 9
   تركيزthe filtrate was concentrated
10. 10
    أخرىpurified with column chromatography (carrier: silica gel, elute: toluene:hexane=1:4)

الإجراء التجريبي

26.28 g (0.15 mol) of 5-(N-acetylamino)indane, 43.61 g (0.20 mol) of p-iodotoluene, 25.88 g (0.188 mol) of anhydrous potassium carbonate and 2.38 g (0.038 mol) of a copper powder were mixed and while introducing a nitrogen gas, the resulting mixture was heated to 20° C. and stirred for 6 hours. After completion of the reaction, 22.3 g of potassium hydroxide dissolved in 20 ml of water and 50 ml of isoamyl alcohol were added to conduct hydrolysis at 130° C. for 2 hours. After completion of the hydrolysis, 250 ml of water was added, and Isoamyl alcohol was removed by azeotropic distillation. 200 ml of toluene was added to dissolve the reaction product. After filtration, the reaction product was dehydrated with magnesium sulfate. After filtering out the magnesium sulfate, the filtrate was concentrated, and purified with column chromatography (carrier: silica gel, elute: toluene:hexane=1:4) to obtain 32.3 of indan-5-yl-p-tolylamine.

المصدر