Reaktion #1483083

Reaktionsgleichung

tetrakis(aminomethyl)methane tetrachloride

NaOMe MeOH

→

tetrakis(aminomethyl)methane

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTetrakis(aminomethyl)methane is prepared by a known procedure (Adil, K. et al., Solid State Sciences, 6 (2004), 1229-1235)
2. 2
   SonstigeA 50 mL flask is equipped with a reflux condenser and a magnetic stirrer
3. 3
   Temperaturrefluxed for 4 hours
4. 4
   Temperaturcooled
5. 5
   SonstigeMethanol solution is decanted from the inorganic salts
6. 6
   Einengenthe combined organics are concentrated in vacuo
7. 7
   workup.DISSOLUTIONThe residue is dissolved in methylene chloride (15 mL)
8. 8
   Filtrationfiltered
9. 9
   Filtration(0.45 micron filter) from the remaining inorganic salts

Vorschrift

Tetrakis(aminomethyl)methane is prepared by a known procedure (Adil, K. et al., Solid State Sciences, 6 (2004), 1229-1235). A 50 mL flask is equipped with a reflux condenser and a magnetic stirrer. The flask is charged with tetrakis(aminomethyl)methane tetrachloride (800 mg, 2.88 mmol), methanol (10 mL) and NaOMe/MeOH solution (2.10 g of 5.457M, 11.50 mmol). The mixture is stirred and refluxed for 4 hours, then cooled. Methanol solution is decanted from the inorganic salts, and the salts are re-suspended in absolute ethanol (15 mL). The suspension is centrifuged, and the combined organics are concentrated in vacuo. The residue is dissolved in methylene chloride (15 mL) and filtered using a syringe (0.45 micron filter) from the remaining inorganic salts. Concentration of the filtrates affords free tetrakis(aminomethyl)methane in a quantitative yield as a white semi-solid material (the residual alcohol is estimated by NMR). NMR (D2O) δ 2.9 (s, CH2)

Quelle