Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A chemical synthesis, methoxy technology, applied in the direction of organic chemistry, can solve the problem of low reaction yield, and achieve the effect of increased yield, large implementation value and social and economic benefits
Active Publication Date: 2009-03-18
ZHEJIANG JIUZHOU PHARM CO LTD
View PDF2 Cites 3 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0011] Like this, in these two routes of above-mentioned A, B, especially use sodium methylate in B route, there is the shortcoming that reaction yield is low
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0023] Add 500ml of methanol into a 1000ml flask, then add 175g of KOH, and heat up to reflux until dissolved. Add 100g of 10,11-dibromoiminodibenzyl, heat and reflux for 24 hours; evaporate methanol to dryness under reduced pressure, add 300ml of water, stir, filter, and dry to obtain 10-methoxy-5H-dibenzo[b,f ] Azapine crude product 48.4g, yield 90.1%;
[0024] Add 48.4 g of the crude product of 10-methoxy-5H-dibenzo[b, f]azepine to 200 ml of methanol, heat to dissolve, cool, crystallize, filter and dry to obtain 10-methoxy-5H-dibenzo[b,f] [b, f] 41.9g of azapine fine product, the refined yield is 78.0%.
Embodiment 2
[0026] Add 500ml of methanol into a 1000ml flask, then add 219g of CH3OK (supplier: Zibo Fuxier Chemical Co., Ltd.), heat up and reflux until dissolved. Add 100g of 10,11-dibromoiminodibenzyl, heat and reflux for 24 hours; evaporate methanol to dryness under reduced pressure, add 300ml of water, stir, filter, and dry to obtain 10-methoxy-5H-dibenzo[b,f ] Azapine crude product 47.1g, yield 87.6%;
[0027] Add 47.1 g of the crude product of 10-methoxy-5H-dibenzo[b, f]azepine to 200 ml of methanol, heat to dissolve, cool, crystallize, filter and dry to obtain 10-methoxy-5H-dibenzo[b,f] [b, f] 40.7g of azapine fine product, the refined yield is 75.7%.
[0028] In summary, the chemical synthesis method of 10-methoxy-5H-dibenzo[b,f]azepine of the present invention has reasonable process, high reaction yield and is suitable for large-scale industrial production.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Login to view more
Abstract
The invention provides a method for chemically synthesizing 10-methoxy-5H-dibenzo[b, f]azepin. The method comprises the following steps: using 10, 11-dibromo-imino-dibenzyl as a raw material to react with potassium hydroxide or potassium methoxide in methanol so to generate the10-methoxy-5H-dibenzo[b, f]azepin; preferably, firstly, adding the potassium hydroxide or the potassium methoxide in the methanol, adding the 10, 11-dibromo-imino-dibenzyl into the mixture after heating up and refluxing the mixture, and reducing the pressure and distilling the methanol after heating up and refluxing the mixture as well as keeping the temperature for a period of time; secondly, adding water into the mixture, and stirring, filtering and drying the mixture to obtain a crude product of the 10-methoxy-5H-dibenzo[b, f]azepin; and finally, adding solvent into the crude product for refinement to obtain the refined product of the 10-methoxy-5H-dibenzo[b, f]azepin. The method has the advantages of reasonable process and high reaction yield, and suitability for large-scale industrial production.
Description
technical field [0001] The present invention relates to the technical field of 10-methoxyl-5H-dibenzo[b,f]azepine, more specifically, relates to the technical field of 10-methoxyl-5H-dibenzo[b,f]azepine The technical field of chemical synthesis, in particular, refers to a chemical synthesis method of 10-methoxy-5H-dibenzo[b,f]azepine. Background technique [0002] 10-methoxy-5H-dibenzo[b,f]azepine (10-methoxy-5H-dibenz[b,f]azepine), molecular formula: C 15 h 13 NO, molecular weight: 223.27, appearance is bright yellow crystalline powder, its structural formula is as follows: [0003] [0004] It is a chemical intermediate and has a very wide range of uses in the fields of chemical and pharmaceutical synthesis. At present, the chemical synthesis methods of 10-methoxy-5H-dibenzo[b,f]azepine mainly contain the following two routes: [0005] A. British Patent GB943277, the announcement date is: December 4, 1963, the name is: dibenzo [b, f] azepines and their preparation p...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
![Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine](https://images-eureka.patsnap.com/patent_img/bc0de548-bc69-4853-94b8-eb36843563e9/a200810201851d00031.PNG)
![Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine](https://images-eureka.patsnap.com/patent_img/bc0de548-bc69-4853-94b8-eb36843563e9/a200810201851d00032.PNG)
![Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine](https://images-eureka.patsnap.com/patent_img/bc0de548-bc69-4853-94b8-eb36843563e9/a200810201851d00041.PNG)
Login to view more 
Login to view more