Cyclen tetrahydrochloride → 1,4,7,10-Tetraazacyclododecane
Reaktionsgleichung
[CH2:1]1[NH:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4][NH:3][CH2:2]1.Cl.Cl.Cl.Cl>C(Cl)(Cl)Cl>[NH:3]1[CH2:4][CH2:5][NH:6][CH2:7][CH2:8][NH:9][CH2:10][CH2:11][NH:12][CH2:1][CH2:2]1Komponenten
3
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ 2.32 (s, 4 H), 2.70 (s, 16 H).
Aufarbeitung
- customwas bubbled NH3 (g) through a gas dispersion tube for 1 hour