반응 #1483083

반응 방정식

tetrakis(aminomethyl)methane tetrachloride

NaOMe MeOH

→

tetrakis(aminomethyl)methane

용매

methanol

반응 조건

후처리

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

실험 절차

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)

출처