Surfactant, preparation method thereof, and related intermediate and its application
A technology for surfactants and amino acids, which is applied in the preparation method thereof and the intermediates involved, in the field of surfactants, achieves the effects of good foaming and emulsifying properties, good biodegradation properties and mild action
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Embodiment 1
[0054] The preparation of embodiment 1 n-butyryl chloride (3a)
[0055]
[0056] In a three-necked flask equipped with a thermometer and a reflux condenser, heat 60 mL of thionyl chloride to reflux, add 89 g of n-butyric acid dropwise, drop it for about 3 hours, then reflux for 2 hours, distill at atmospheric pressure, and collect fractions at 100-105 ° C. About 100 g of n-butyryl chloride (3a) was obtained.
Embodiment 2
[0057] The preparation of embodiment 2N-n-butyryl glutamic acid (5a)
[0058]
[0059] In a dry 1L three-necked flask, add 16.9g of sodium glutamate and 60mL of water, cool in an ice-salt bath to about 0-5°C, adjust the pH value to 10.5 with 20% aqueous sodium hydroxide solution, and slowly add the solution prepared in Example 1 dropwise. The obtained n-butyryl chloride was 10.6g, and kept the internal temperature at 0-5°C, dripped for about 2.5h, continued to stir for 1.5h, removed the ice-water bath, naturally warmed to room temperature, continued the reaction for 1h, and then cooled to 0-5°C, After adjusting the pH value to 3-4, a large amount of solids were precipitated, filtered by suction, and dried to obtain 20.5 g of N-n-butyryl glutamic acid (5a) as a white powdery solid.
Embodiment 3
[0060] The preparation of embodiment 3N-n-butyrylglutamyl chloride (6a)
[0061]
[0062] In a dry 1L round bottom flask, add 12.5g of N-n-butyrylglutamic acid (5a), 60mL of thionyl chloride, and a catalytic amount of DMF, and react at 40-50°C for 6-8h until no acidic gas escapes to obtain Brown solution, excess thionyl chloride was distilled off under reduced pressure to obtain 12.1 g of n-butylglutamyl chloride (6a).
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