Supercharge Your Innovation With Domain-Expert AI Agents!

Method for continuously producing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine

A technology of hydroxyethylamine and ethyl, which is applied in the field of continuous production of 5--2-pentylamine, can solve the problems of cumbersome operation steps, excessive waste discharge, serious environmental pollution, etc., and achieve improved economic benefits and low catalyst cost , good life stability

Active Publication Date: 2020-07-31
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, the Raney nickel catalyst used in the reductive amination reaction of 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentanone in the first and second methods is made of nickel aluminum alloy in strong Made by dissolving aluminum under alkali, there is serious environmental pollution, and the catalyst is deactivated and lost during use
In addition, the process adopts a batch production method, which has low production efficiency and a lot of waste discharge
Although the third method is a non-ammonation and non-catalytic hydrogenation process, the operation steps are cumbersome and the production cycle is long, and the reduction of the ketone carbonyl group in the esterification product needs to use expensive borohydride reagents, so the production cost is high and there are many wastes

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
  • Method for continuously producing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine
  • Method for continuously producing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine
  • Method for continuously producing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] In some more specific embodiments, adopt co-precipitation method or deposition precipitation method to prepare and obtain described loaded nano-nickel-based catalyst; The preparation method of described loaded-type nano-nickel-based catalyst comprises:

[0033] Mix the mixed metal salt solution containing the main active component and the auxiliary agent, the lye with the metal salt solution of the carrier, the carrier oxide powder solution, and the carrier colloid particle solution at a pH of 9.5-10 A precipitation reaction occurs, followed by aging treatment at 30-100°C for 2-24h, then roasting at 400-800°C for 2-10h, and then reduction treatment at 400-750°C for 2-8h in a reducing atmosphere to obtain the supported Nano-nickel-based catalysts.

[0034] Further, the lye includes any one or a combination of two or more in sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, potassium carbonate solution, and is not limited thereto.

[003...

Embodiment 1

[0046] 66.88g Ni(NO 3 ) 2 ·6H 2 O, 2.17g Cu(NO 3 ) 2 ·3H 2 O, 117.0g Al(NO 3 ) 3 9H 2 O was added into 1100ml deionized water successively to prepare a 0.5mol / L metal salt solution A; 40g NaOH and 21.2g NaOH 2 CO 3 Add 200ml of deionized water to make a mixed alkaline solution B; add salt solution A and alkaline solution B dropwise to a 2000ml three-necked flask at the same time under rapid stirring, keep the pH of the precipitation process = 10±0.2, and raise the temperature to 80°C after the precipitation is completed After aging for 4 hours, filter after aging, and wash with deionized water until the filtrate is neutral. The filter cake was dried at 110°C for 12h and calcined at 400°C for 10h. Tablet sieve 20-40 mesh catalyst particles, fill 4g in a fixed-bed reactor, heat up to 550°C for 4 hours in a hydrogen atmosphere (flow rate 100mL / min) and reduce for 4 hours to obtain activated catalyst 1, the composition of the catalyst and the active metal Ni The grain s...

Embodiment 2

[0048] 60.45g NiSO 4 ·6H 2 O, 8.71g CoSO 4 ·7H 2 O, 95.97g Al 2 (SO 4 ) 3 18H 2 O is added to 810ml deionized water successively to prepare metal salt solution A of 0.5mol / L; the preparation of mixed alkali solution B and catalyst precipitation is the same as in Example 1; Wash with water until the filtrate is neutral. The filter cake was dried at 110°C for 12h and calcined at 500°C for 6h. Tablet sieve 20-40 mesh catalyst particles, fill 4g in a fixed bed reactor, heat up to 500°C and reduce for 6h in a hydrogen atmosphere (flow rate 100mL / min) to obtain activated catalyst 2, the composition of the catalyst and the active metal Ni The grain sizes are listed in Table 1. Weigh 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentanone, ethanol, and 25% concentrated ammonia water in a mass ratio of 1:1:3 to prepare a reaction solution. At a reaction temperature of 120°C, H 2 Pressure 0.2MPa, H 2 The molar ratio to 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentanone is 5:1 and the feed ...

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

No PUM Login to View More

Abstract

The invention discloses a method for continuously producing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine, and the method comprises the following steps: in a reducing atmosphere, continuously inputting a mixed solution containing 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentanone and a nitrogen source into a fixed bed reactor filled with a supported nano nickel-based catalyst; carrying out reductive amination reaction under the conditions that the pressure is 0.2 to 2MPa, the temperature is 80 to 140 DEG C and the feeding mass space velocity is 0.2 to 1.0 h <-1 >, so as to prepare the 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine. According to the method provided by the invention, the continuous production of the 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine can be realized under theaction of the supported nano Ni catalyst and a nitrogen source; meanwhile, the catalyst is low in cost, high in production efficiency, good in stability, simple to operate, low in production cost andconvenient for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical intermediate synthesis, in particular to a method for continuously producing 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine. Background technique [0002] Hydroxychloroquine sulfate tablet, its chemical name is: 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl]ethylamino]-ethanol sulfate, molecular formula is: C 18 h 26 ClN 3 O·H 2 SO 4 , the molecular weight is 433.96, and the chemical structural formula is as follows: [0003] [0004] Hydroxychloroquine sulfate belongs to 4-aminoquinoline antimalarial drugs, consisting of two aromatic rings, one ethyl group in chloroquine is replaced by a hydroxyethyl group, it is a derivative of chloroquine phosphate, its structure and mechanism of action are similar to chloroquine phosphate , has better safety, and can replace chloroquine phosphate in clinical practice. With the application of antimalarials in the treatment of systemic lupus erythema...

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
no application Login to View More
IPC IPC(8): C07C215/14C07C213/02B01J23/755B01J23/83B01J23/889B01J23/825
CPCC07C213/02B01J23/755B01J23/83B01J23/8892B01J23/825B01J23/002C07C2523/755C07C2523/83C07C2523/889C07C2523/825B01J35/40C07C215/14
Inventor 黄志威李雪梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com