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A kind of halogen hydrolysis method of pharmaceutical intermediate

A kind of halogen and drug technology, applied in the field of organic synthesis, can solve the problems of discarded resources, compound can not be reused, waste, etc., achieve high product conversion rate, be beneficial to large-scale industrial production, and improve the effect of utilization

Active Publication Date: 2017-11-17
NANJING OCEAN PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the previous process, the compound represented by formula III could not be reused, but could only be discarded, resulting in a waste of resources

Method used

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  • A kind of halogen hydrolysis method of pharmaceutical intermediate
  • A kind of halogen hydrolysis method of pharmaceutical intermediate
  • A kind of halogen hydrolysis method of pharmaceutical intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Hydrolysis of Compound II and Compound III (R group in Compound II and Compound III is Cl)

[0023] Add compound II and compound III (total 3.93g, 10mmol), 10ml water into a 100ml reaction flask, stir and mix, then raise the temperature to reflux at 100°C, the system gradually clarifies during the heating process, and stir for 2h. Spot the plate to detect the complete reaction of the raw material.

[0024] 20ml of dichloromethane extraction system was added to the system, the dichloromethane layer was dried, and the dry solvent was recovered under reduced pressure to obtain 3.7g of compound I with a yield of 98.8%.

Embodiment 2

[0026] Hydrolysis of Compound II and Compound III (R group in Compound II and Compound III is Br)

[0027] Add compound II and compound III (total 8.74g, 20mmol), 20ml water into a 100ml reaction flask, stir and mix, then raise the temperature to reflux at 100°C, the system gradually clarifies during the heating process, and stir for 2h. Spot the plate to detect the complete reaction of the raw material.

[0028] Add 40ml of dichloromethane extraction system to the system, dry the dichloromethane layer, and recover the dry solvent under reduced pressure to obtain 7.36g of compound I with a yield of 98.3%.

Embodiment 3

[0030] Hydrolysis of Compound II and Compound III (R group in Compound II and Compound III is Br)

[0031] Add Compound II and Compound III (6.56g in total, 15mmol), 15ml of water into a 100ml reaction flask, add silver carbonate (1.24g, 4.5mmol) and stir and mix, then heat up to 40°C. During the heating process, the system is gradually clarified and stirred. 2h. Spot the plate to detect the complete reaction of the raw material.

[0032] Add 30 ml of dichloromethane extraction system to the system, dry the dichloromethane layer, and recover the dry solvent under reduced pressure to obtain 5.55 g of compound I with a yield of 98.8%.

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Abstract

The invention discloses a drug intermediate halogen hydrolysis new method, and belongs to the field of chemical synthesis. The hydrolysis method comprises that a hydrolysis reaction is carried out in the presence of solvent water. The hydrolysis method provided by the invention not only greatly improves the raw material utilization ratio, reduces production of organic solid waste, saves the reaction cost, besides, has extremely simple and convenient reaction operations, has high product conversion rate, and is beneficial for industrialized mass production.

Description

technical field [0001] The present invention provides a method for obtaining compound I by hydrolyzing the compound represented by formula II and its spatial isomer compound represented by formula III. This method provides a novel recovery route, which has the characteristics of low cost, less by-products and high yield. Specifically related to the field of organic synthesis. Background technique [0002] The compound represented by the formula I is an important raw material for preparing the compound represented by the pharmaceutical intermediate formula II. During the preparation of the compound represented by the formula II, the compound represented by its stereoisomer formula III will be produced. However, in the previous process, the compound represented by formula III could not be reused, but could only be discarded, resulting in a waste of resources. [0003] [0004] Wherein, the R group can be a series of halogen groups such as Cl and Br. Contents of the inv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/18C07H1/00
CPCC07H1/00C07H15/18
Inventor 陈本顺
Owner NANJING OCEAN PHARMA TECH