BATCH PROCESS FOR THE PREPARATION OF CIS-2,2,4,4-TETRAMETHYLCYCLOBUTANE-1,3-DIOL

摘要

This invention is generally directed to a batch process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol comprising: (A) treatment of at least one monomer selected from 2,2,4,4- tetramethylcyclobutane-1,3-dione, 3-hydroxy-2, 2,4,4- tetramethylcyclobutanone, and 2,2,4,4-tetramethylcyclobutane-1,3-diol said diol having a starting cis:trans molar ratio of 0:1 to about 2:1, or mixtures thereof by contacting said monomer(s) with hydrogen in the presence of a reaction solvent in which the resulting cis-2, 2,4,4- tetramethylcyclobutane-1,3-diol is partially soluble and further in the presence of a catalyst comprising about 0.1 to about 10 weight percent ruthenium, based on the total weight of the catalyst, deposited on a support material, under reaction conditions sufficient to produce a cis- 2,2,4,4-tetramethylcyclobutane-1,3-diol having a final cis:trans molar ratio of from 2:1 to about 25:1; (B) removal of the reaction solvent, whether by filtration, centrifugation, or other methods known to one of ordinary skill in the art; (C) dissolution of the 2,2,4,4-tetramethylcyclobutane-1,3-diol with at least one solvent; and, optionally, (D) washing the catalyst at least once, and optionally, (E) reuse of the catalyst.