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2,6,7-Trioxa-1-borabicyclo[2.2.2]octan-3-one, 4-methyl- synthesis

2synthesis methods
-

Yield:1188369-88-1 100%

Reaction Conditions:

in ethanol;

Steps:

3

EXAMPLE 3 13.061 g of ethyl borate B(OC2H5)3 are added, in 75 ml of 95% ethanol, to 12 g of commercially available 2,2-bis(hydroxymethyl)propionic acid CH3C(CH2OH)2CO2H, with magnetic stirring. The clear solution obtained is evaporated under vacuum on a rotary evaporator and the drying is continued under a primary vacuum at 75° C. The syrupy mass is converted into a white solid which is isolated (quantitative yield) and corresponds to the formula CH3C[(CH2O-)2(CO2-)]B (IB-3). 6 g of this complex are dissolved in 25 ml of anhydrous dimethylformamide (DMF) and a clear solution is obtained. 2.46 g of potassium fluoride dried at 150° C. under a primary vacuum are added. KF, which is strictly insoluble in DMF, goes into solution rapidly so as to form the adduct K+{CH3C[(CH2O-)2(CO2-)BF}-.

References:

US2011/171112,2011,A1 Location in patent:Page/Page column 13