Electric Literature of 91893-69-5, A common heterocyclic compound, 91893-69-5, name is 2-Amino-N,N-dimethylethanesulfonamide hydrochloride, molecular formula is C4H13ClN2O2S, its 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.
General procedure: General procedure C: A mixture of amine hydrochloride (1.73 mmol), NaOH (0.10 g, 2.59 mmol) and ethanol (50 mL) was stirred and heated to reflux for 1 h. Then gossypol acetic acid (0.50 g, 0.86 mmol) was added and the reaction liquid continued to reflux for 5 h. The reaction mixture was cooled to room temperature and then the resulting solid was filtered, washed with ethanol and then recrystallized with pyridine and ethanol or chloroform and ethanol to give the desired gossypol derivatives. Data for 19: General procedure C; yellow solids; yield, 61.0%; mp, 235-237C; 1H NMR (400MHz, CDCl3) delta 13.47-13.37 (m, 2H), 9.64 (d, J=12.2Hz, 2H), 7.89 (s, 2H), 7.59 (s, 2H), 5.61 (s, 2H), 3.95 (dd, J=11.8, 6.5Hz, 4H), 3.76-3.66 (m, 2H), 3.26 (t, J=6.5Hz, 4H), 2.88 (s, 12H), 2.11 (s, 6H), 1.55-1.50 (m, 12H); 13C NMR (100MHz, CDCl3) delta 173.51, 162.80, 149.02, 146.96, 132.25, 129.22, 128.09, 118.37, 115.97, 114.40, 103.70, 48.57, 45.17, 37.28, 27.45, 20.34, 20.29, 20.07; HRMS (ESI) calcd for C38H49N4O10S2 (M-H)- 785.2896, found 785.2873.
The synthetic route of 91893-69-5 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Li, Ling; Li, Zheng; Wang, Kailiang; Liu, Yuxiu; Li, Yongqiang; Wang, Qingmin; Bioorganic and Medicinal Chemistry; vol. 24; 3; (2016); p. 474 – 483;,
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