Lipopeptide molecule surfactant containing azobenzene photosensitive group, and synthetic method thereof
The technology of surfactant and photosensitive group is applied in the field of chemical synthesis of lipopeptide molecules, which can solve the problems of excessive reaction raw materials, high product price, low conversion rate, etc., and achieves simple separation and purification method, high synthesis efficiency and purity, The effect of reducing product waste
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[0036] 1. Synthesis of intermediate azobenzenecarboxylic acid (compound 3):
[0037]
[0038] ① 4-n-hexylaniline (14.18g, 80mmol) was dissolved in 45mL HCl (540mmol) and 120mL H 2 In the mixed solution of O, stir for 30min under ice-bath conditions, until the solution turns into a tan suspension;
[0039] ②NaNO 2 (5.53g, 80mmol) was dissolved in 30mL H 2 In O, drop into the above-mentioned reaction system with a dropping funnel while stirring (2s / drop), and continue to stir and react for 20min under ice-bath conditions until the solution gradually becomes clear;
[0040] ③Phenol (7.53g, 80mmol), Na 2 CO 3 (21.17g, 200mmol) was dissolved in 120mL H 2 Form an emulsion in O, and drop it into the above solution with a dropping funnel while stirring (2 s / drop), bubbles are generated in the solution, and a large amount of yellow solid precipitates are gradually formed.
[0041] ④ After the reaction is complete, take a small amount of sample and analyze it by thin-layer chro...
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