Acetic Acid → HCID 54488712, compound

Participants

Reaction Steps

As described in Example 1, a mixture of 37.6 g of bis-(tetrahydrofurfuryl) phosphite and 4.9 g of mesityl oxide in 80 ml of benzene was reacted by heating in the presence of 1.3 g of sodium over the course of 1 hour. The reaction was vigorously exothermic. The sodium was neutralized by addition of 3.4 g of glacial acetic acid. The inorganic salt was extracted from the mixture with 2 portions of 20 ml of water. The benzene solvent was removed in a rotary evaporator, leaving as residue 32.6 g of crude product which still contained di-tetrahydrofurfuryl phosphite. Distillation of 4.3 g of the crude product in a bulb tube oven in high vacuum yielded the desired product at an oven temperature between 185° C. and 230° C. and a pressure of 0.01 mm Hg.

Provenance & Evidence