Sodium methanolate methanol → 4742-00-1

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)

1. customTetrakis(aminomethyl)methane is prepared by a known procedure (Adil, K. et al., Solid State Sciences, 6 (2004), 1229-1235)
2. customA 50 mL flask is equipped with a reflux condenser and a magnetic stirrer
3. temperaturerefluxed for 4 hours
4. temperaturecooled
5. customMethanol solution is decanted from the inorganic salts
6. concentrationthe combined organics are concentrated in vacuo
7. dissolutionThe residue is dissolved in methylene chloride (15 mL)
8. filtrationfiltered
9. filtration(0.45 micron filter) from the remaining inorganic salts

ORD record

ord-6ecc1ae838194197ba30f52697dac998

Source dataset

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08460696B2