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Preparation method of polysubstituted benzo nitrogen-containing heterocyclic methylamine

An extraction and extraction device technology, which is applied in the field of preparation of pharmaceutical intermediates, can solve the problems of inconvenient vibration operation of the extraction device, difficulty in the implementation of the extraction process, and small volume of the extraction device, so as to solve the problem of demulsification, sufficient fixing strength and high yield. high effect

Active Publication Date: 2020-12-25
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

[0006] The first purpose of the present invention is to solve two specific problems in the prior art, one is to set out from aceguvaldehyde dimethyl acetal, how to obtain 3-methylisoquinoline 8-methylamine through few steps with high yield again The problem of this application perfectly solves the problem. The second is that it is difficult to implement the extraction process, the volume of the extraction device is too small, and the vibration operation of the extraction device is too large, which is obtained in this application. solved

Method used

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  • Preparation method of polysubstituted benzo nitrogen-containing heterocyclic methylamine
  • Preparation method of polysubstituted benzo nitrogen-containing heterocyclic methylamine
  • Preparation method of polysubstituted benzo nitrogen-containing heterocyclic methylamine

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Embodiment 1

[0052] An ultrasonic extraction device is characterized in that it includes an extraction part 1 , a shell part 2 , an ultrasonic part 3 , a bar part 4 , a left support part 5 , a right support part 6 , a glassware 7 and an emulsion breaking component 8 . The extraction device can be divided into multiple specifications, for example, the volume of the extraction part can be 1L, 2L, 3L, 4L, 5L to meet different needs.

[0053] The extraction part 1 includes a cylindrical part 11 , an upper opening 12 , an upper cover 13 , a cone part 14 , a stopper set 15 and a liquid outlet 16 . The main part of the extraction part 1 is spliced ​​from top to bottom by an upper opening 12, a cylindrical part 11, and a cone part 14. The cylindrical part 11 is a hollow cylinder, the upper opening 12 is large and the bottom is small, and the inner surface is a frosted part. 121, the outer edge of the upper cover 13 adapted to the frosted part 121 is a frosted surface, the upper center of the upper...

Embodiment 2

[0062] A method for preparing multi-substituted benzonitrogen-containing heterocyclic methylamines is performed using an ultrasonic extraction device as described above due to the large amount of extraction required, and is characterized in that it includes the following steps.

[0063] (1) Dissolve 64-68g of acetone aldehyde dimethyl acetal in 1900-2100ml of toluene, add 105-115g of o-bromobenzylamine under stirring, heat up to about 120 degrees Celsius, react until the water separation is complete, and confirm that the reaction is complete by LCMS detection, Concentration gave N-(2-bromophenyl)-1,1-dimethoxypropan-2-imine as a light yellow liquid.

[0064] (2) Dissolve 165-175g of N-(2-bromophenyl)-1,1-dimethoxypropane-2-imine in 1600-1800ml of ethanol, and control the temperature to below 30-35 degrees Celsius, Slowly add 55-59g of sodium borohydride in batches. After the addition is complete, continue to react at 30-35 degrees Celsius for 8-16h. Confirm the reaction is com...

Embodiment 3

[0069] A method for preparing multi-substituted benzonitrogen-containing heterocyclic methylamines is performed using an ultrasonic extraction device as described above due to the large amount of extraction required, and is characterized in that it includes the following steps.

[0070] (1) Dissolve 68g of acetone aldehyde dimethyl acetal in 2100ml of toluene, add 113.33g of o-bromobenzylamine under stirring, raise the temperature to about 120 degrees Celsius, react until the water separation is complete, confirm the reaction is complete by LCMS detection, and concentrate to obtain a light yellow liquid N-(2-bromophenyl)-1,1-dimethoxypropan-2-imine. Yield 100%.

[0071] (2) Dissolve 175g of N-(2-bromophenyl)-1,1-dimethoxypropan-2-imine in 1800ml of ethanol, control the temperature below 32 degrees Celsius, and slowly add 59g of Sodium borohydride, after the addition is complete, continue to react at 32 degrees Celsius for 10 hours, confirm the reaction is complete by LCMS, ad...

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Abstract

The invention relates to a preparation method of polysubstituted benzo nitrogen-containing heterocyclic methylamine, which is carried out by using an ultrasonic extraction device and is characterizedby comprising the steps of preparing N-(2-bromophenyl)-1, 1-dimethoxypropane-2-imine from pyruvic aldehyde dimethyl acetal and o-bromobenzylamine; and preparing a red viscous oily matter 3-methylisoquinoline-8-methylamine through four steps to obtain a final product. The extraction is implemented by an ultrasonic extraction device, and comprises a preparation step, a covering step, a vibration shaking step, a repeating step and a receiving step. The ultrasonic extraction device comprises an extraction part (1), a shell part (2), an ultrasonic part (3), a transverse rod part (4), a left supporting part (5), a right supporting part (6), a glass device (7) and a demulsification assembly (8).

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a preparation method of polysubstituted benzonitrogen-containing heterocyclic methylamines. Background technique [0002] Isoquinoline and its derivatives are an important class of compounds with strong biological activity and are widely used in medicine, pesticides and other fields. Therefore, the synthesis of pyrazole derivatives has received extensive attention, especially in pharmaceutical intermediates is widely used. A kind of preparation method of 8-nitro-1,2,3,4-tetrahydroisoquinoline is given in CN2016100987718, and a kind of synthesis of 4-hydroxyl-8-bromoisoquinoline is given in CN201610042580.X Method, a preparation method of 7-bromoisoquinoline is given in CN201210340505.3, which are examples of the application and synthesis of isoquinoline derivatives, but the 3-methylisoquinoline 8 mentioned in this application - Methylamine is...

Claims

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Application Information

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IPC IPC(8): B01D11/04B01J19/10C07D217/02
CPCB01D11/0423C07D217/02
Inventor 马强
Owner 烟台宁远药业有限公司
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