TRIETHANOLAMINE BORATE synthesis

Yield: 70%

Reaction Conditions:

in water at 120;

Steps:

1 Synthesis of Silatrane Via Boratrane
To a 25 mL flask was added boric acid (50 mmol) and triethanolamine (50 mmol). Water (3 mL) was added to facilitate solubility. The flask was equipped with a short path distillation apparatus and heated to 120° C. until no more water condensed. The isolated boratrane was recrystallized from acetonitrile and used directly in the next step. The experimental data collected are in agreement with those described in the literature.[1] 70%. 1H NMR (500 MHz, CDCl₃): δ=3.65 (t, J=5.5 Hz, 6H), 3.04 (t, J=5.5 Hz, 6H). 13C NMR (125 MHz, CDCl₃) 62.1, 59.3. IR (ATR) 2988, 2853, 1469, 1370, 1258, 1160, 1115, 1063, 1026, 1001, 933, 889, 730, 621, 560.

References:

Board of Trustees of Northern Illinois University;Adler, Marc J.;Gilbert, Thomas M.;Varjosaari, Sami E.;Skrypai, Vladislav US2017/362151, 2017, A1 Location in patent:Paragraph 0073-0074