ChemicalBook CAS DataBase List DOTA

DOTA synthesis

12synthesis methods

Product Name:DOTA
CAS Number:60239-18-1
Molecular formula:C16H28N4O8
Molecular Weight:404.42

3926-62-3 Synthesis

3926-62-3
258 suppliers
$19.73/250g

294-90-6 Synthesis

294-90-6
512 suppliers
$5.00/1g

60239-18-1
287 suppliers
$9.00/250mg

Yield:60239-18-1 92.1%

Reaction Conditions:

in acetonitrile; for 6 h;Inert atmosphere;Reflux;

Steps:

10.4 Step (4): Preparation of compound 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) of formula 7

Keeping a slight positive pressure of nitrogen, 3L of acetonitrile and 149.02g (0.865mol) of the compound of formula 5 were added to the 5L reaction flask, and 477.57g (4.1mol) of sodium chloroacetate was added to it in batches with stirring. After the addition, the temperature was raised to reflux for reaction. The reaction was maintained under reflux for 6 hours, and the reaction was completed. The reaction solution was cooled to room temperature, filtered, and the filtrate was rotary evaporated to recover the solvent. The residue was recrystallized with an appropriate amount of toluene-acetonitrile (2:1, v/v) to obtain 323.32 g (0.797 mol) of white solid product. The yield is 92.1%, the total yield of the four-step reaction is 79.7%, Product titration purity: 99.7% (by HClO4),

References:

CN113956262,2022,A Location in patent:Paragraph 0177-0178; 0192-0197