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Formation of dimethylbenzenediol via acyloin condensation and a reduction-oxidation pathway

Technical Report ·
OSTI ID:6024412

Interest with benzenediol formation was initiated by the isolation and identification of 2,5-dimethyl-1,4-benzenediol from the liquefaction product of cellulose. During that same work 2,5-dimethyl-2,5-cyclohexadiene-1,4-dione(1), 2,3-butadione (biacetyl) and 3-hydroxy-2-butanone (acetoin) were also detected as liquefaction products under aqueous alkaline conditions. Several alkylbenzenediols have been isolated as alkaline degradation products of xylose and glucose, while 1 was observed after alkali treatment of sucrose. Early work had indicated that both 1 and 2,5-methyl-1,4-benzenediol, (2), could be prepared by warming 10g of biacetyl in 200 ml of dilute caustic solution. However, yield information was given only for the product of 2,3-pentadione (10% of 2,5-diethyl-2,5-cyclohexadiene-1,4-dione). Results with biacetyl under similar conditions suggested that the yields of 1 and 2 were in the 1 to 5% range depending upon reaction time; i.e. 0.75 hr was required for 1% 1 while 4 hrs were required for 5% 1. When acetoin was subjected to similar conditions neither 1 or 2 were detected during the initial 4 hr.

Research Organization:
Pacific Northwest Lab., Richland, WA (USA)
DOE Contract Number:
AC06-76RL01830
OSTI ID:
6024412
Report Number(s):
PNL-SA-10350(2); ON: DE85005527
Country of Publication:
United States
Language:
English