Electric Literature of 5395-50-6,Some common heterocyclic compound, 5395-50-6, name is 1,3,4,6-Tetrakis(hydroxymethyl)tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, molecular formula is C8H14N4O6, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
1 ,3,4,6-tetrakis(hydroxymethyl)tetrahydroimidazo [4,5-d]imidazole-2,5(1H,3H)-dione (1.88 g, 7.2 mmol) in 1.5 ml of DMSO was dissolved. Then, 0.15 ml nitric acid (65%) and n-l3uOH (13.12 ml, 143 mmol) were added to the solution and the mixture was heated at 60 C. for 16 hours. After the reaction was over, the reaction liquid was cooled and iN NaOH was added around pH 7. Around 100 ml ethyl acetate was used to extract with mixture and the organic phase was washed by saturated NaC1(aq) solution for 2 times. After being dried by Na2504, the solvent was removed. The crude compound was purified by flash chromatography (Heptane/EtOAc). The product was obtained colorless viscous oil in 0.38 g, yield (11%) ?H NMR (600 MHz, DMSO-d6): oe (ppm) 5.52 (s, 2H), 4.73 (m, 8H), 3.35 (m, 8H), 1.46 (m, 8H), 1.29 (m, 8H), 0.85 (t, 12H)
The synthetic route of 5395-50-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Rohm and Haas Electronic Materials LLC; Rohm and Haas Electronic Materials Korea Ltd.; Grandbois, Matthew; Kim, Myung Yeol; Ryu, Eui Hyun; Sim, Jae Hwan; Jang, Min Kyung; Lee, Jung-June; (17 pag.)US2017/59991; (2017); A1;,
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