反应 #1797494

反应方程式

5-(N-acetylamino)indane

p-iodotoluene

potassium carbonate

potassium hydroxide

→

indan-5-yl-p-tolylamine

溶剂

water

water

isoamyl alcohol

反应条件

后处理

1. 1
   workup.ADDITIONwhile introducing a nitrogen gas
2. 2
   其他hydrolysis at 130° C. for 2 hours
3. 3
   workup.ADDITIONwas added
4. 4
   其他Isoamyl 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
   过滤After filtration
8. 8
   过滤After filtering out the magnesium sulfate
9. 9
   浓缩the filtrate was concentrated
10. 10
    其他purified with column chromatography (carrier: silica gel, elute: toluene:hexane=1:4)

实验过程

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.

来源