反应详情

温度

200 °C

5-(N-Acetylamino)indane (26.28 g (0.15 mol)), 43.61 g (0.20 mol) of iodotoluene, 25.88 g (0.188 mol) of anhydrous potassium carbonate and 2.38 g (0.038 mol) of copper powder were mixed, and heated up to 200° C. while introducing nitrogen gas, followed by stirring for 6 hours. After the termination of the reaction, cooling was conducted, and 22.3 g of potassium hydroxide dissolved in 20 ml of water and 50 ml of isoamyl alcohol were added to perform hydrolysis at 130° C. for 2 hours. After the termination of the hydrolysis, 250 ml of water was added, and isoamyl alcohol was removed by azeotropic distillation. Then, 200 ml of toluene was added to dissolve the reaction product. After filtration, dehydration was performed with magnesium sulfate. After magnesium sulfate was removed by filtration, the filtrate was concentrated, and purified by column chromatography (carrier: silica gel, eluent: toluene:hexane 1:4) to obtain 32.3 g of indane-5-yl-p-tolylamine.

1. additionwhile introducing nitrogen gas
2. customAfter the termination of the reaction
3. temperaturecooling
4. customhydrolysis at 130° C. for 2 hours
5. additionwas added
6. customisoamyl alcohol was removed by azeotropic distillation
7. additionThen, 200 ml of toluene was added
8. dissolutionto dissolve the reaction product
9. filtrationAfter filtration, dehydration
10. customAfter magnesium sulfate was removed by filtration
11. concentrationthe filtrate was concentrated
12. custompurified by column chromatography (carrier: silica gel, eluent: toluene:hexane 1:4)