Preparation method of 1-substituted taurine
A technology of taurine and xanthate, applied in the field of preparation of 1-position substituted taurine, can solve the problems of troublesome desalination and purification process, many steps and the like
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Embodiment 1
[0043] Preparation of 1-phenyl-2-aminoethylsulfonic acid (3a)
[0044] Dissolve 5.42 g (20 mmol) of O-ethyl dithiocarbonate S-(1-phenyl-2-nitroethyl) ester in formic acid (12 mL), and add H 2 o 2 (2.4mL), keep the reaction temperature at 0-5°C and stir the reaction overnight. After the reaction is completed, the solvent is distilled off to obtain 1-phenyl-2-nitroethylsulfonic acid.
[0045] Dissolve the obtained 1-phenyl-2-nitroethylsulfonic acid in methanol, add 60 mg of 10% palladium carbon, reduce it with hydrogen under stirring, evaporate the solvent, and recrystallize with ethanol to obtain colorless crystal 1- Phenyl taurine 2.33g, yield 58%, melting point 352°C (dec). 1 H NMR (D 2 O, 200MHz) (δ, ppm): 3.54 (dd, J=8.4, 13.3Hz, 1H in CH 2 N), 3.76(dd, J=6.8, 13.3Hz, 1H in CH 2 N), 4.27(dd, J=6.8, 8.4Hz, 1H, CHS), 7.38(s, 5H, ArH). 13 C NMR (DMSO-d 6 , 50MHz) (δ, ppm): 40.9, 61.5, 127.2, 127.9, 129.0, 136.1.
Embodiment 2
[0047] Preparation of 1-(4-methylphenyl)-2-aminoethylsulfonic acid (3b)
[0048] According to the method described in Example 1, use O-ethyl dithiocarbonate S-[1-(4-methylphenyl)-2-nitroethyl] ester as raw material to obtain 1-(4-methyl Phenyl)-2-aminoethylsulfonic acid, colorless crystals, melting point 339-342°C, yield 60%. 1 H NMR (D 2 O, 300MHz) (δ, ppm) 2.24 (s, 3H, CH 3 ), 3.49 (dd, J=8.4, 13.3Hz, 1H in CH 2 N), 3.71(dd, J=6.8, 13.3Hz, 1H in CH 2 N), 4.21 (dd, J=6.8, 8.4Hz, 1H, CHS), 7.19 (d, J=8.4Hz, 2H, ArH), 7.24 (d, J=8.4Hz, 2H, ArH). 13 C NMR (D 2 O, 75.5MHz) (δ, ppm) 20.9, 40.8, 63.1, 129.5, 129.6, 130.3, 140.3.
Embodiment 3
[0050] Preparation of 1-(4-chlorophenyl)-2-aminoethyl-1-sulfonic acid (3c)
[0051] According to the method described in Example 1, use dithiocarbonic acid O-ethyl ester S-[1-(4-chlorophenyl)-2-nitroethyl] ester as raw material to obtain 1-(4-chlorophenyl )-2-aminoethylsulfonic acid, colorless crystals, melting point 342°C, yield 67%. 1 H NMR (D 2 O, 300MHz) (δ, ppm) 3.47 (dd, J=8.7, 13.4Hz, 1H in CH 2 N), 3.76(dd, J=6.9, 13.4Hz, 1H in CH 2 N), 4.27 (dd, J=6.9, 8.4Hz, 1H, CHS), 7.38 (m, 4H, ArH). 13 C NMR (D 2 O, 75.5MHz) (δ, ppm) 41.1, 61.9, 129.2, 129.4, 130.9, 134.9.
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