反応 #2459027

反応方程式

hydrogen

Pyridine-2-carboxaldehyde

1,5,9-triazanonane

hydrogen

→

1,11-Bis(2-pyridyl)-2,6,10-triazaundecane

溶媒

ethanol

反応条件

後処理

1. 1
   その他the charcoal catalyst was removed by filtration, and dry HCl gas
2. 2
   その他was bubbled into the solution until no further white precipitate
3. 3
   その他formed
4. 4
   その他After removing the precipitate
5. 5
   ろ過by filtration of the cooled solution
6. 6
   洗浄the product was washed with absolute ethanol
7. 7
   その他dried
8. 8
   その他recrystallized from 95% ethanol

実験手順

Pyridine-2-carboxaldehyde (4.3 g, 0.04 mole) and 1,5,9-triazanonane (2.6 g, 0.02 mole) [bis(aminopropyl)- amine; available from Aldrich Chemical Company] were dissolved in ca. 60 ml of absolute ethanol and warmed (ca. 50° C.) with stirring for 10 minutes. The solution was hydrogenated at room temperature over 1.5 g of 5% Pd on charcoal in an atmosphere of hydrogen. After the calculated amount of hydrogen (0.04 mole; ca. 0.90 1 at 25° C. and 1 atm. pressure) had been consumed, the charcoal catalyst was removed by filtration, and dry HCl gas was bubbled into the solution until no further white precipitate formed. After removing the precipitate by filtration of the cooled solution, the product was washed with absolute ethanol, dried, and recrystallized from 95% ethanol.

出典