2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of Methyl 2,2,2-trichloroacetimidate
A round-bottom 3 neck flask was charged with 3,4-diaminobenzenesulfonic acid (8.0 g, 42.5 mmol) and anhydrous MeOH (0.85 L). O-Methyl-1,1,1-trichloroacetimidat was added (2.8 mL, 3.74 g, 21.2 mmol). The resultant suspension was stirred for 24 h at ambient conditions. Additional amount of O-methyl-1,1,1-trichloroacetimidat was added (1.4 mL, 1.87 g, 10.5 mmol) after this time, then reaction mixture was stirred for 72 h days at ambient conditions, heated for 3 h at 50 C. and triethylamine (14 mL, 9.4 g, 93.5 mmol) was added. Stirring was continued at this temperature for 18 h. Then reaction mixture was cooled to 30 C., and an intensive flow of dry HCl was passed through the solution until a precipitate formed. The suspension was filtered off at 40 C., precipitate was washed with MeOH (4×150 mL, stirring of suspension for 10-15 min each turn) and with MeOH-HCl 3.5% solution (100 mL, 1 h of stirring). Product 1H,1’H-2,2′-bibenzimidazole-5,5′-disulfonic acid was pale yellow or colorless, weight 3.5 g, yield 42%. It may contain own hydrochloride as a salt. NMR1 H spectrum (Brucker Avance 300 instrument; solvent d6-dimethyl sulfoxide; delta, ppm; J, Hz): 5.27 br.s (-SO3H in exchange with H2O and NH) 7.73 m (2Ha,2Hb), 8.01 br.s (2Hx). NMR 13C{1H} spectrum (Brucker Avance 300 instrument; solvent d6-dimethyl sulfoxide; delta, ppm): 113.00, 115.41, 123.27, 136.44, 137.60, 142.24, 145.34.
The synthetic route of 2533-69-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CRYSOPTIX KK; US2010/279122; (2010); A1;,
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