Jackpot-OTC SYNTHESIS!!!!!!
Al/Hg reduction of Oxylic acid to glyoxylic acid
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Glyoxylic acid.
Dukai, Jozsef; Varkonyi-Rozsa, Agnes; Barath, Mrs. Miklos. (Chinoin Gyogyszer es Vegyeszeti Termekek Gyara Rt., Hung.). Hung. Teljes (1979), 20 pp. CODEN: HUXXBU HU 15960 19790127 Patent written in Hungarian.
Patent No.
HU 15960
HU 173712
Abstract
X:CHCO2H (X = O, H2NCONHN, and H2NCSNHN) and 2-hydroxyquinoxaline were prepd. by Hg or Hg2+ activated Al redn. of oxalic acid (I). Thus, a mixt. of 2.5 L MeOH, 35 g 99.5% Al turnings, and 10 mL 1% HgCl2 in MeOH was stirred 10-15 min, stirred 6 h at 20-30° with 296 g I, kept overnight, filtered, and the MeOH replaced by H2O. The soln. was passed through Varion KS (H+) cation-exchange resin, concd. at 40-50° to deposit unreacted I, and filtered to give a soln. contg. 75-80 g glyoxylic acid.
This one might bee even better.
Glyoxalic acid.
(Daicel Chemical Industries, Ltd., Japan). Jpn. Kokai Tokkyo Koho (1983), 6 pp. CODEN: JKXXAF JP 58198437 A2 19831118 Showa. Patent written in Japanese.
Abstract
OHCCO2H (I) was prepd. by reaction of aq. oxalic acid (II) with Cl. Thus, Cl was introduced to 1850.2 g aq. soln. contg. 5.03% II and 0.48% I over 19 h at 15-18° to give 1984.3 g aq. soln. contg. 5.08% I. Conversion of II and selectivity for I were 92.8% and 83.4%, resp.
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