Method for preparing substituted taurine
A technology of taurine and sulfuric acid, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as lack of further development and application, unfavorable substitution reactions, and lack of raw materials
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Embodiment 1
[0055] Preparation of (S)-2-amino-3-phenylpropylsulfonic acid (1a)
[0056] (1) Esterification:
[0057]A mixture of ice-cold 4g concentrated sulfuric acid and 4mL water was added under cooling in an ice-water bath into a 50mL round-bottomed flask containing 6.05g (40mmol) (S)-2-amino-3-phenyl-1-propanol and 4mL water, Heating to 120-130°C with stirring, and distilling off the water under reduced pressure to obtain a colorless or slightly yellow solid or oily aminoalcohol sulfuric acid monoester. Colorless crystals can be obtained after recrystallization from ethanol, but purification is generally not required.
[0058] (2) replace:
[0059] Dissolve the sulfuric acid monoester obtained above in 80 mL of water, add 7.56-10.08 g (60-80 mmol) of sodium sulfite, and stir and react at 0-100° C. for 12-72 hours. The solvent was distilled off, and the residue was recrystallized from methanol or a mixture of methanol and ether to obtain a colorless crystalline product, substituted...
Embodiment 2
[0061] Preparation of (S)-2-amino-2-phenylethylsulfonic acid (1b)
[0062] According to the method described in Example 1, (S)-2-amino-2-phenylethylsulfonic acid was obtained from (S)-2-amino-2-phenylethanol as a colorless crystal with a melting point of 332°C , The two-step total yield is 30-69%. [α] D 20 = -1.3 (c 1.00, HCO 2 H). 13 CNMR (50MHz, HCO 2 H)δ: 57.6, 62.7, 127.4, 129.4, 129.9, 132.8.
Embodiment 3
[0064] Preparation of (S)-3-methyl-2-amino-butylsulfonic acid (1c)
[0065] According to the method described in Example 1, (S)-3-methyl-2-aminobutanol was used as raw material to obtain (S)-3-methyl-2-amino-butylsulfonic acid, colorless crystals, melting point 325~326℃, two-step total yield 70%.[α] D 20 =+29.7(c1.01, HCO 2 H). 13 CNMR (75.5 MHz, HCO 2 H)δ: 16.2, 17.1, 30.3, 49.3, 54.6.
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