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Preparation method of 3-nitro-4-fluorophenylacetate

A technology of fluorophenylacetate and fluorophenylacetate, which is applied in the field of preparation of 3-nitro-4-fluorophenylacetate, can solve the problems of low conversion rate of raw materials, poor spatial position selectivity, etc., and achieves safety High performance, control the heat release problem, and avoid the effect of rapid heat dissipation

Active Publication Date: 2020-02-18
暨明医药科技(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is that in the method for preparing 3-nitro-4-fluorophenylacetic acid ester from 4-fluorophenylacetic acid ester in the prior art, there are technologies such as low raw material conversion rate and poor spatial position selectivity. question

Method used

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  • Preparation method of 3-nitro-4-fluorophenylacetate
  • Preparation method of 3-nitro-4-fluorophenylacetate
  • Preparation method of 3-nitro-4-fluorophenylacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Preparation of raw materials: Take 200 g of ethyl 4-fluorophenylacetate and dissolve it in 280 mL of 98% sulfuric acid for later use. Take 79mL69% nitric acid for use.

[0035] (2) Pre-cooling: cool down the pre-cooling module and mixing module to 0-10°C. Use two constant flow pumps to pump the sulfuric acid solution and nitric acid solution of ethyl 4-fluorophenylacetate into two parallel pre-cooling modules for cooling to 0-10°C.

[0036] (3) Mixing: After the pre-cooling of the raw materials is completed, they enter the mixing module for mixing reaction. The flow rate of the mixed solution of 4-fluoroethyl phenylacetate and concentrated sulfuric acid is set to 15mL / min, and the flow rate of nitric acid is 2.63mL / min. The reaction stays in the mixing module 42s.

[0037] (4) Quenching and post-processing: the reaction liquid enters the quenching tank for quenching, and there are 500 mL of ethyl acetate and 500 mL of water in the quenching tank. The reaction sol...

Embodiment 2-9

[0039] The preparation method is the same as in Example 1, and the amount of ethyl 4-fluorophenylacetate is fixed at 200 g, the difference lies in the amount of raw materials and some process parameters. At the same time, in order to ensure that the mixed solution of 4-fluorophenylacetate and concentrated sulfuric acid and the nitric acid solution entering the mixing module of the microreactor can fully participate in the reaction, the flow rate is also changed as required. The products after the reaction are denoted as S2-S9.

Embodiment 10

[0042] (1) Preparation of raw materials: Take 185 g of methyl 4-fluorophenylacetate and dissolve it in 280 mL of 98% sulfuric acid for later use. Take 79mL69% nitric acid for use.

[0043] (2) Pre-cooling: cool down the pre-cooling module and mixing module to 0-10°C. Use two constant flow pumps to pump the sulfuric acid solution and nitric acid solution of methyl 4-fluorophenylacetate into two parallel pre-cooling modules for cooling to 0-10°C.

[0044] (3) Mixing: After the raw materials are pre-cooled, they enter the mixing module for mixing reaction. The flow rate of the mixed solution of methyl 4-fluorophenylacetate and concentrated sulfuric acid is set to 14.8mL / min, and the flow rate of nitric acid is 2.63mL / min. React in the mixing module Stay for 42s.

[0045] (4) Quenching and post-processing: the reaction liquid enters the quenching tank for quenching, and there are 500 mL of ethyl acetate and 500 mL of water in the quenching tank. The reaction solution was quench...

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Abstract

The invention discloses a method for preparing 3-nitro-4-fluorophenylacetate by using a microreactor, and belongs to the technical field of organic matter synthesis, the microreactor comprises precooling modules and a mixing module, and the method specifically comprises the following steps: (1) preparing raw materials: preparing a mixed solution of 4-fluorophenylacetate and concentrated sulfuric acid and a nitric acid solution; (2) pre-cooling: cooling the pre-cooling modules and the mixing module to a reaction temperature in advance, and then respectively adding the mixed solution of 4-fluorophenylacetate and concentrated sulfuric acid and the nitric acid solution into different pre-cooling modules; (3) mixing: after the raw materials are pre-cooled, adding the pre-cooled raw materials into the mixing module for mixing reaction; and (4) performing quenching and post-processing. The method provided by the invention can effectively control the heat release problem of the nitration reaction, and is high in safety; and the 3-nitro-4-fluorophenylacetate can be prepared with high selectivity, the conversion rate of the 4-fluorophenylacetate can reach 98.4%, and the selectivity can reach99: 1.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a preparation method of 3-nitro-4-fluorophenylacetate. Background technique [0002] Dihydronaphthyridines are a class of kinase inhibitors for the treatment or prevention of diseases such as gastrointestinal stromal tumors, acute myeloid leukemia and systemic hypertrophy. And when constructing dihydronaphthyridines, 3-nitro-4-fluorophenylacetate is an important intermediate, but the method for synthesizing 3-nitro-4-fluorophenylacetate is comparatively complicated and also fresh. There are literature reports. [0003] A kind of 4-fluorobenzene Ethyl acetate is used as a raw material, and the method for obtaining ethyl 3-nitro-4-fluorophenylacetate through nitration reaction, the specific preparation process is the nitration reaction carried out in a traditional reaction bottle. The outstanding feature of nitrification reaction is strong exotherm...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/56
CPCC07C201/08C07C205/56
Inventor 陈剑戈李斌峰苑可
Owner 暨明医药科技(苏州)有限公司
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