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Method for preparing nitrate ester compound by adopting micro-flow field reaction technology

A technology for compounds and nitrates, which is applied in the field of preparing nitrate compounds by using microfluidic field reaction technology, can solve the problems of intractable treatment of acid wastewater, inability to enlarge industrially, expensive equipment investment, etc., and achieves easy post-processing, improved safety, The effect of shortening the reaction time

Active Publication Date: 2018-02-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The technical problem to be solved in the present invention is to provide a method for preparing nitrate ester compounds using micro-flow field reaction technology, so as to solve the problems of difficult separation of reactions, difficult treatment of acid wastewater, low reaction efficiency, inability to scale up in industry and equipment problems in the prior art. Problems such as expensive investment, realize the synthesis of nitrate compounds with high yield and high selectivity without using strong acid and high-cost catalyst

Method used

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  • Method for preparing nitrate ester compound by adopting micro-flow field reaction technology
  • Method for preparing nitrate ester compound by adopting micro-flow field reaction technology
  • Method for preparing nitrate ester compound by adopting micro-flow field reaction technology

Examples

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Effect test

Embodiment 1

[0052] 2-Phenyl-4,5-dihydrooxazole (2mmol, 1.0eq) and TBN (6mmol, 3.0eq) were respectively dissolved in 20mL 1,4-dioxane. Take the prepared solvent and load it in a syringe, and pump it into the microchannel modular reaction device. The reaction solution was reacted at 80°C, and the reaction time was 2h. The reaction solution flowing out of the microchannel modular reaction device was poured into saturated sodium sulfite solution (30mL), extracted with ethyl acetate (50mL×3), and the combined organic layer was washed with anhydrous Na 2 SO 4 Dry, filter, and evaporate the solvent in a vacuum to obtain a crude product. Recrystallize the crude product with ethanol to obtain a pure product with a yield of 95%.

Embodiment 2

[0056] 2-(p-methylphenyl)-4,5-dihydrooxazole (2mmol, 1.0eq) and TBN (6mmol, 3.0eq) were dissolved in 20mL of 1,4-dioxane. Take the prepared solvent and load it in a syringe, and pump it into the microchannel modular reaction device. The reaction solution was reacted at 80°C, and the reaction time was 2h. The reaction solution flowing out of the microchannel modular reaction device was poured into saturated sodium sulfite solution (30mL), extracted with ethyl acetate (50mL×3), and the combined organic layer was washed with anhydrous Na 2 SO 4 Dry, filter, and evaporate the solvent in a vacuum to obtain a crude product. The crude product is recrystallized from ethanol to obtain a pure product with a yield of 91%.

Embodiment 3

[0060] Dissolve 2-(4-chlorophenyl)-4,5-dihydrooxazole (2mmol, 1.0eq) and TBN (6mmol, 3.0eq) in 20mL 1,4-dioxane respectively. Take the prepared solvent and load it in a syringe, and pump it into the microchannel modular reaction device. The reaction solution was reacted at 80°C, and the reaction time was 2h. The reaction solution flowing out of the microchannel modular reaction device was poured into saturated sodium sulfite solution (30mL), extracted with ethyl acetate (50mL×3), and the combined organic layer was washed with anhydrous Na 2 SO 4 Dry, filter, and evaporate the solvent in a vacuum to obtain a crude product. Recrystallize the crude product with ethanol / flash column chromatography to obtain a pure product with a yield of 85%.

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Abstract

The invention discloses a method for preparing a nitrate ester compound by adopting a micro-flow field reaction technology. The method comprises the following steps: dissolving an oxazole compound andtert-butyl nitrite into an organic solvent to obtain a mixed solution; pumping the obtained mixed solution into a micro-channel modular reaction device for reaction to prepare the nitrate ester compound. The micro-channel modular reaction device comprises a micro-structure mixer, a micro-structure reactor and a product collector which are sequentially connected with each other through pipelines,and temperature in the micro-structure reactor is controlled by a micro-heat exchanger. According to the method provided by the invention, a conventional nitrification method for preparing the nitrateester compound is changed, and the use of concentrated sulfuric acid and concentrated nitric acid is avoided; moreover, the method has the advantages of simple production device, easiness for processcontrol, easiness for wastewater treatment and the like.

Description

Technical field [0001] The invention belongs to the technical field of chemical synthesis, and specifically relates to a method for preparing nitrate compounds by adopting a microfluidic field reaction technology. Background technique [0002] Nitrate compounds can stimulate endogenous nitric oxide to produce nitric oxide synthase and cytochrome P450 substrates by releasing nitric oxide. This mechanism of action has established the important position of nitrate compounds in the pharmaceutical industry. Nitrate compounds mainly have anti-inflammatory and analgesic effects and blood vessel expansion. Nitrate compounds with anti-inflammatory and analgesic effects mainly include NO-indomethacin, NO-ibuprofen and NO-acetylsalicylic acid, etc. In the treatment of cardiovascular diseases, the more important drugs are mainly nitroglycerin, isosorbide and nicorandil. [0003] [0004] Currently, there are generally two methods for preparing nitrate compounds. The first method shown in Rou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/67C07C231/10C07D213/82C07D307/68C07D333/38C07D213/81B01J19/00
CPCB01J19/0093C07C231/10C07D213/81C07D213/82C07D307/68C07D333/38C07C233/67
Inventor 郭凯袁鑫方正乔凯万力何伟郑明卫欧阳平凯
Owner NANJING UNIV OF TECH
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