As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 517-21-5, name is Sodium 1,2-dihydroxyethane-1,2-disulfonate, molecular formula is C2H4Na2O8S2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. name: Sodium 1,2-dihydroxyethane-1,2-disulfonate
Glyoxal-sodium bisulfite (2.72 g, 10.2 mmol) was added to a solution of 3-amino-5-methyl-1H-pyrazole (2 g, 20.6 mmol) in water (40 mL) and was heated to 70 C. for 25 min. The mixture was then cooled down to room temperature and sodium cyanoborohydride (2.73 g, 43.4 mmol) was added and the mixture was stirred overnight. Methanol (70 mL) was added and the mixture was stirred for 1 h. Concentrated hydrochloric acid (12 N) was added until a pH<2 was obtained and the resulting mixture was stirred at room temperature overnight. The solution was then neutralized with an aqueous solution of sodium hydroxide (1M) and the solvent was evaporated. The residue was resuspended in methanol (40 mL) and stirred for 1 h. After filtration, the solvent was evaporated and the residue was purified by chromatography on a silica gel column (eluent: EtOAc, EtOAc-MeOH, 95:5, 90:10); N1,N2-bis(5-Methyl-1H-pyrazol-3-yl)ethane-1,2-diamine was obtained as a white solid.1H NMR (400 MHz, CDCl3): delta=2.21 (s, 6H), 3.35 (s, 4H), 5.35 (s, 2H).13C NMR (100 MHz, CDCl3/CD3OD 10:1): delta=11.29, 43.86, 89.75, 142.32, 155.13.MS (ESI): m/z=221 (MH+).
With the rapid development of chemical substances, we look forward to future research findings about 517-21-5.
Reference:
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