反应详情

温度

50 °C

111 g (1.5 moles) of 1,3-diaminopropane and 300 g of fully dehydrated isopropyl ether were weighed in an atmosphere of nitrogen into a 2-liter three-necked round-bottomed flask equipped with a cooling condenser and stirrer. With sufficient stirring, 237 g (0.59 mole) of perfluorohexyl sulfonyl fluoride was added dropwise at room temperature from a dropping funnel. The mixture was stirred at 50° C. for 3 hours, and then the isopropyl ether was removed under reduced pressure. The oily residue was dissolved in 200 ml of ethanol, and gradually poured into 5 liters of distilled water with stirring. The resulting crystals were aged. The supernatant liquid was removed by decantation, and 1 liter of 0.5 N aqueous sodium hydroxide solution was added to wash the crystals. Decantation was performed for three more times using 5 liters of distilled water each time. The crystals were collected by filtration, washed with distilled water and dried at 60° C. under reduced pressure. There was obtained 268 g of N-(3 -aminopropyl)perfluorohexyl sulfonamide having a sufficient purity for use in the subsequent reaction.

1. customequipped with a cooling condenser and stirrer
2. customthe isopropyl ether was removed under reduced pressure
3. dissolutionThe oily residue was dissolved in 200 ml of ethanol
4. additiongradually poured into 5 liters of distilled water
5. stirringwith stirring
6. customThe supernatant liquid was removed by decantation, and 1 liter of 0.5 N aqueous sodium hydroxide solution
7. additionwas added
8. washto wash the crystals
9. filtrationThe crystals were collected by filtration
10. washwashed with distilled water
11. customdried at 60° C. under reduced pressure