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Low-temperature continuous synthesis device and method for medical intermediate halogenated isoquinoline boric acid

A technology of bromoisoquinoline and boronic acid, which is applied in the field of low-temperature continuous synthesis devices for pharmaceutical intermediates halogenated isoquinoline boronic acids, and can solve problems such as danger

Pending Publication Date: 2022-01-04
烟台宁远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is very dangerous to perform this reaction batchwise

Method used

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  • Low-temperature continuous synthesis device and method for medical intermediate halogenated isoquinoline boric acid
  • Low-temperature continuous synthesis device and method for medical intermediate halogenated isoquinoline boric acid
  • Low-temperature continuous synthesis device and method for medical intermediate halogenated isoquinoline boric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]A continuous reaction device is characterized in that it includes a first feeder, a second feeder, a third feeder, a continuous reactor, a first pump, a second pump, a third pump, and a product container.

[0030] The continuous reactor has a first inlet, a second inlet, a third inlet and a reactor outlet, and the coil volume in the continuous reactor is not less than 30ml.

[0031] The inlet pipe connected to the inlet of the first pump is inserted into the first feeder, the outlet pipe connected to the outlet of the first pump is connected to the first inlet; the inlet pipe connected to the inlet of the second pump is inserted into the second feeder, and the outlet pipe connected to the outlet of the first pump is connected to the first inlet; The outlet pipe connected to the outlet of the second pump is connected to the second inlet; the inlet pipe connected to the inlet of the third pump is inserted into the third feeder, and the outlet pipe connected to the outlet of...

Embodiment 2

[0035] A preparation method of 3-chloroisoquinoline boronic acid series is characterized in that it comprises the following steps.

[0036] (1) raw material preparation step: control the temperature at 20 ° C, add 10 g of 3-chloro-5-bromoisoquinoline at a rate of 0.4 g / min and dissolve it in 100 ml of concentrated sulfuric acid to obtain the first raw material, Keep nitrogen atmosphere and put it into the first feeder.

[0037] The control system is at -70°C, every 10g of 3-chloro-5-bromoisoquinoline is matched with 32ml of n-butyllithium and 120ml of fuming sulfuric acid, and 32ml of n-butyllithium is added dropwise at a speed of 0.4ml / min In oleum of 120ml, obtain the second raw material, keep the nitrogen atmosphere and put it into the second feeder.

[0038] The control system is at 20°C, every 10g of 3-chloro-5-bromoisoquinoline is matched with 15g of trimethyl borate and 19ml of tetrahydrofuran, 15g of trimethyl borate is added at a rate of 0.4g / min and dissolved in 20m...

Embodiment 3

[0043] A preparation method of 3-chloroisoquinoline boronic acid series is characterized in that it comprises the following steps.

[0044] (1) raw material preparation step: control the temperature at 20°C, add 10g of 3-chloro-5-bromoisoquinoline at a rate of 0.45g / min and dissolve it in 105ml of concentrated sulfuric acid to obtain the first raw material, Keep nitrogen atmosphere and put it into the first feeder.

[0045] The control system is at -72°C, every 10g of 3-chloro-5-bromoisoquinoline is matched with 33ml of n-butyllithium and 125ml of fuming sulfuric acid, and 33ml of n-butyllithium is added dropwise at a speed of 0.45ml / min In oleum of 125ml, obtain the second raw material, keep nitrogen atmosphere and put it into the second feeder.

[0046] The control system is at 22°C, every 10g of 3-chloro-5-bromoisoquinoline is matched with 16g of trimethyl borate and 21ml of tetrahydrofuran, 16g of trimethyl borate is added at a rate of 0.45g / min and dissolved in 21ml In ...

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Abstract

The invention provides a continuous reaction device. The continuous reaction device comprises a first feeder, a second feeder, a continuous reactor, a first pump, a second pump, a product container, a third pump and a third feeder, wherein the continuous reactor is provided with a first inlet, a second inlet, a third inlet and an outlet; the first feeder, the second feeder, the third feeder and the product container are polytetrafluoroethylene containers; and the first feeder, the second feeder and the third feeder are positioned in a nitrogen atmosphere. The invention also discloses a synthesis method of 3-chloroisoquinoline boric acid series compounds. The method is carried out by using the continuous reaction device.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a low-temperature continuous synthesis device and method for pharmaceutical intermediates of halogenated isoquinoline boronic acids. Background technique [0002] The 3-chloroisoquinoline boronic acid series is an important class of compounds with strong biological activity and is widely used in the fields of medicine, pesticides and other fields. The 3-chloroisoquinoline-8-boronic acid mentioned in this application is rarely used as a The application of pharmaceutical intermediates appears, or literature or information is published. Due to the characteristics of the molecule, the unique synthetic route, and the unique higher yield problem, this method cannot be extended to the synthesis of other similar structures. [0003] Due to the properties of this molecule, this method cannot be extended to the synthesis of other similar structures. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J4/00C07F5/02
CPCB01J4/001B01J4/008C07F5/025
Inventor 刘杰杰苏德泳蔡艳林智杰姚焱民
Owner 烟台宁远药业有限公司