Reference of 115-20-8, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.115-20-8, name is Trichloroethanol, molecular formula is C2H3Cl3O, molecular weight is 149.4, as common compound, the synthetic route is as follows.
A solution of 3-tert-butyl-5-methylsulfamoyl-benzoic acid (WO 2008/021388, which is incorporated herein by reference in its entirety, 400 mg, 1.47 mmol) in THF (10 ml) was treated with TEA (270 mu1, 1.91 mmol) and DPPA (412 mul, 1.91 mmol). The reaction mixture was stirred at RT for 1 hour and then 2,2,2-trichloro-ethanol (225 mul, 2.35 mmol) was added. The reaction mixture was heated at 70 C. for 18 hours and cooled at RT. The volatiles were removed under reduced pressure and the residue was partitioned between EtOAc and an aqueous 5% citric acid solution. The two phases were separated and the aqueous phase was extracted with EtOAc. The combined organic phases were washed with a saturated aqueous NaHCO3 solution and brine, dried with Na2SO4 and the solvent was removed under reduced pressure. Purification by FCC, eluting with 0-70% EtOAc/cyclohexane gave the title compound (429 mg, 70%). 1H NMR (300 MHz, CDCl3): 1.35 (9H, s), 2.69 (3H, d, J=5.4 Hz), 4.45 (1H, q, J=5.4 Hz), 4.84 (2H, s), 7.18 (1H, br s), 7.62 (1Ht, J=1.7 Hz), 7.66 (1H, br s), 7.81 (1H, br s).
Statistics shows that 115-20-8 is playing an increasingly important role. we look forward to future research findings about Trichloroethanol.
Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; CAPALDI, Carmelida; ARMANI, Elisabetta; JENNINGS, Andrew Steven Robert; HURLEY, Christopher; (82 pag.)US2017/183345; (2017); A1;,
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