Tetraethylammonium bis[salicylato-(2-)]borate synthesis

Yield:3765-12-6 80%

Reaction Conditions:

with boric acid in water at 100; for 0.25 h;Heating / reflux;

Steps:

19 EXAMPLE 19; Synthesis of tetraethylammonium bis(salicyl)borate

1 mole of tetraethylammonium hydroxide (35% in water), 1 mole of boric acid and 2 moles of salicylic acid were mixed in 200 ml water and heated to boiling. At 100° C. two liquid phases had formed after 15 minutes, then it was cooled to room temperature and allowed to settle. The lower layer was collected by decantation and washed with water, and then cooled to 4° C. overnight. The product was isolated in 80% yield. It remained a liquid while in contact with water, however when the water was removed a higher melting point solid (m.p. 117-119° C.) was obtained. The hydrate was unstable towards loss of water at 4° C.

References:

US2004/7693,2004,A1 Location in patent:Page 5