Process intensification-assisted conversion of alpha,omega-alkanediols to dibromides

作者：Mekala Shekar; Hahn Roger C^*

来源：Tetrahedron Letters, 2015, 56(4): 630-632.

DOI：10.1016/j.tetlet.2014.11.132

• Process intensification
• Azeotrope fractionation
• alpha,omega-Diol to dibromide
• Scalable reaction

The increasingly widespread applications of alpha,omega-dibromides motivated development of a scalable, inexpensive process to rapidly convert selected alpha,omega-alkanediols to the corresponding dibromides. Diols were heated with only 48% aq HBr and an organic solvent, using a Dean-Stark apparatus modified to fractionate the azeotropic distillate, thereby maintaining a higher HBr concentration and reaction rate in the pot. Intensified distillation also increased the reaction rate. Various other substrate, solvent, and parameter effects have been discovered and rationalized.

• 出版日期2015-1-21