A method for continuous production of 5-(n-ethyl-n-2-hydroxyethylamine)-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 excessive waste discharge, cumbersome operation steps, serious environmental pollution, etc., and achieve improved economic benefits and simple reaction process High efficiency and low catalyst cost

Active Publication Date: 2022-02-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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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

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  • A method for continuous production of 5-(n-ethyl-n-2-hydroxyethylamine)-2-pentylamine
  • A method for continuous production of 5-(n-ethyl-n-2-hydroxyethylamine)-2-pentylamine
  • A method for continuous production of 5-(n-ethyl-n-2-hydroxyethylamine)-2-pentylamine

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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 ...

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Abstract

The invention discloses a method for continuously producing 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine. It includes: in a reducing atmosphere, the mixed solution containing 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentanone and a nitrogen source is continuously input and loaded with a loaded nano-nickel-based catalyst In the fixed-bed reactor, the pressure is 0.2-2MPa, the temperature is 80-140℃, and the mass space velocity of the feed is 0.2-1.0h ‑1 Reductive amination reaction is carried out under certain conditions, and 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine is obtained. The method provided by the invention can realize the continuous production of 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine under the action of loaded nano-Ni catalyst and nitrogen source; simultaneously the catalyst in the present invention The method has low cost, high production efficiency, good stability, simple operation, low production cost and is convenient for industrialized 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

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/14C07C213/02B01J23/755B01J23/83B01J23/889B01J23/825
CPCC07C213/02B01J23/755B01J23/83B01J23/8892B01J23/825B01J23/002B01J35/023C07C2523/755C07C2523/83C07C2523/889C07C2523/825C07C215/14
Inventor 黄志威李雪梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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