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Method for synthesizing beta-brominated alcohol by anisotropic emulsion microreactor

An anisotropic, micro-reactor technology, applied in the field of chemistry, can solve problems such as limitations

Active Publication Date: 2021-07-23
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing emulsion reaction system is limited in the field of material synthesis

Method used

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  • Method for synthesizing beta-brominated alcohol by anisotropic emulsion microreactor
  • Method for synthesizing beta-brominated alcohol by anisotropic emulsion microreactor
  • Method for synthesizing beta-brominated alcohol by anisotropic emulsion microreactor

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Effect test

Embodiment 1

[0027] The volume ratio of oil to water is 1:1, and the volume ratio of FC-770 / n-heptane is changed to a-4:1; b-2:1; c-1:1; d-1:2; e-1:4 . Shake for 3 min under this condition to prepare the emulsion.

[0028] Authentication: from image 3 It can be seen that the volume ratio of FC-770 / n-heptane can form an emulsion under the conditions of 4:1; 2:1; 1:1; 1:2; 1:4, but the emulsion formed under the condition of the volume ratio of 4:1 is One-sided emulsion, while other volume ratios are anisotropic emulsions. With the decrease of the volume of FC-770 in the initial oil phase and the increase of the volume of n-heptane phase, the volume of FC-770 domains in the droplet also decreases gradually, and the volume of n-heptane domains gradually increases. The volume ratio of FC-770 / n-heptane domains can be varied from 4:1 to 1:4.

Embodiment 2

[0031] Keep 2wt% Tween 80 (aq) : n-heptane: FC-770 volume ratio is 2:1:1. Shake for 3 min under this condition to prepare the emulsion. Micrographs of droplets were taken under online temperature control at different temperatures. Sudan I dyes dissolve selectively in the n-heptane phase.

[0032] Authentication: from Figure 4 It can be seen that the temperature has an effect on the type of droplets. As the temperature increases to 45℃, the type of droplets changes from anisotropic emulsion to single-sided emulsion, and the anisotropy of the emulsion disappears.

Embodiment 3

[0035] Keep the aqueous phase:n-heptane:FC-770 volume ratio at 2:1:1. Wherein the surfactant aqueous solution is respectively a-2wt% Tween 80, b-1wt% Tween 80+0.31wt% FS-30, c-0.6wt% Tween 80+0.43wt% FS-30, d-0.62wt% FS- 30. Fluorescent dyes are selectively dissolved in the n-heptane phase. Shake for 3 min under this condition to prepare the emulsion.

[0036] Authentication: from Figure 5 It can be seen that the type of surfactant can affect the topology of the emulsion. With the decrease of Tween 80 and the increase of FS-30 in the water phase, the topology of the emulsion changes from F / H / W to H / F / W.

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Abstract

The invention discloses a method for synthesizing beta-brominated alcohol by an anisotropic emulsion microreactor. Anisotropic emulsion liquid drops are used as a micro-reactor, reaction raw materials, namely olefin and N-bromosuccinimide (NBS), are selectively dissolved in an n-heptane phase and a surfactant aqueous solution phase which are mutually insoluble respectively, fluorocarbon oil is selected as a third phase, an anisotropic emulsion with fluorocarbon oil / n-heptane as an internal phase and a surfactant aqueous solution as an external phase is prepared by a one-step vortex oscillation method; two reaction raw materials are selectively solubilized and isolated by a multi-phase microcell of anisotropic emulsion droplets, meanwhile, the characteristics of multi-phase interfaces and multi-microstructures of the anisotropic droplets are fully exerted, so that static controllable synthesis of beta-brominated alcohol is realized without continuous stirring. The method has the advantages of simplicity and convenience in operation, low energy consumption, controllable reaction rate and easiness in product recovery.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for synthesizing β-bromoalcohol with an anisotropic emulsion microreactor. Background technique [0002] Bromoalcohols are important organic synthons in drug synthesis. Bromoalcohols are used to synthesize aminoalcohols, hydroxy acids and many other widely used intermediates in drug synthesis. Therefore, the development of efficient synthesis methods of bromoalcohols is one of the hot research fields in the current academic and industrial circles. Among the numerous synthesis methods of bromoalcohols, the bromohydroxylation reaction of alkenes is the most direct method for the synthesis of bromoalcohols (Sels B, et al. Nature.400, (1999), 855-857). Existing methods for synthesizing bromoalcohols are still limited by the need to use equivalent metal reagents such as AgNO 3 , HgO, ZnCl 2 And CuO, etc. to activate the addition reaction. These activating reagents are highly toxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/46C07C29/64B01J19/00
CPCC07C29/64B01J19/0093C07C33/46
Inventor 葛玲玲徐德华梁石悦蔡金鹏王海松郭荣
Owner YANGZHOU UNIV
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