The following is a novel synthesis method for GBL.
excerpt:
In to a 100 ml round-bottomed double necked flask containing, THF (0.02 mol, 1.44g), 50% aq. hydrogen peroxide (0.06 mol, 4.08g) and Se02 ( 15mol%, 0.22g).
The reaction was continued with vigorous stirring at 35 oc for 15h. The reaction mixture was then filtered through a Buckner funnel, passed through a short column of silica gel to remove the catalyst and concentrated under reducedpressure.
The resulting residue was analyzed by high resolution GCMSD, El, quadrapole mass analyzer, EM detector. The conversion of THF to GBL was determined on the basis of the weight of the residue left after evaporation and selectivity for GBL formation was determined by GC. Based on these analyses,the conversion of THF was found to be 88 % with the 100 % selectivity for the formation of GBL.
excerpt:
In to a 100 ml round-bottomed double necked flask containing, THF (0.02 mol, 1.44g), 50% aq. hydrogen peroxide (0.06 mol, 4.08g) and Se02 ( 15mol%, 0.22g).
The reaction was continued with vigorous stirring at 35 oc for 15h. The reaction mixture was then filtered through a Buckner funnel, passed through a short column of silica gel to remove the catalyst and concentrated under reducedpressure.
The resulting residue was analyzed by high resolution GCMSD, El, quadrapole mass analyzer, EM detector. The conversion of THF to GBL was determined on the basis of the weight of the residue left after evaporation and selectivity for GBL formation was determined by GC. Based on these analyses,the conversion of THF was found to be 88 % with the 100 % selectivity for the formation of GBL.