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Catalyst for hydrogenation reaction of donepezil hydrochloride key intermediate and application thereof

A technology of donepezil hydrochloride and hydrogenation reaction, applied in metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the problem of high cost of palladium carbon catalyst, and achieve easy control of operating conditions , stable activity and high product yield

Active Publication Date: 2010-04-14
CANGZHOU SENARY CHEM SCI TEC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantages are: the cost of palladium carbon catalyst is higher

Method used

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  • Catalyst for hydrogenation reaction of donepezil hydrochloride key intermediate and application thereof

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Experimental program
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Effect test

Embodiment 1

[0014] Embodiment 1: Catalyst Pd / Al is prepared by impregnation method 2 o 3

[0015] 30g of palladium nitrate was heated and dissolved in 100ml of 1% nitric acid aqueous solution, and 100g of γ-Al was added 2 o 3 , stirred evenly, soaked overnight, dried in a drying oven at 110°C for 20h, roasted in a muffle furnace at 550°C for 5h, and reduced with hydrogen at 400°C and 1.0MPa for 2h to obtain the desired catalyst. The weight composition of the catalyst is: Contains palladium 12.3%, contains Al 2 o 3 87.7%.

Embodiment 2

[0016] Embodiment 2: Catalyst Ni / Al is prepared by impregnation method 2 o 3

[0017] Heat and dissolve 60g of nickel nitrate in 100ml of deionized water, add 100g of γ-Al 2 o 3 , stirred evenly, impregnated overnight, dried in a drying oven at 110°C for 20h, roasted in a muffle furnace at 550°C for 5h, and reduced with hydrogen at 400°C and 1.0MPa for 2h to obtain the desired catalyst. The weight composition of the catalyst is 12.4% nickel, containing Al 2 o 3 87.6%.

Embodiment 3

[0018] Embodiment 3: Catalyst Pd-Ni / Al is prepared by kneading and extruding method 2 o 3

[0019] Heat and dissolve 30g of palladium nitrate and 15g of nickel nitrate in 120ml of 1% nitric acid aqueous solution by mass percentage, add 100g of γ-Al 2 o 3 Powder, fully ground until completely mixed evenly, extruded, dried in a drying oven at 110°C for 20h, roasted in a muffle furnace at 550°C for 5h, reduced with hydrogen at 400°C and 1.0MPa for 2h to obtain the desired catalyst. The weight composition of the catalyst is 11.8% palladium, 3.0% nickel, Al 2 o 3 85.2%.

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Abstract

The invention discloses a catalyst for hydrogenation reaction of a donepezil hydrochloride key intermediate and application thereof. The key intermediate is 2-(1-benzyl-4-piperidine methylene)-5,6-dimethoxy-1-indenone. The catalyst takes Al2O3 as a carrier and comprises composite active components selected from one or several simple substances or the simple substances and oxides of Pd, Cu, Co, Ni, Zn, Fe and Cr, wherein the mass content of each active component is 1-15 percent of the total mass of the catalyst and the total content of the active components is 5-30 percent of the total mass of the catalyst. The catalyst is prepared by utilizing a conventional catalyst preparation method and has the characteristics of low cost, stable activity and cycle use. The hydrogenation reaction by applying the catalyst has the characteristics of easy control of operation conditions, good catalyst performance and high product yield.

Description

technical field [0001] The present invention relates to a hydrogenation technology for a key intermediate of donepezil hydrochloride, especially a key intermediate for donepezil hydrochloride - 2-(1-benzyl-4-piperidinyl methylene)-5,6-di Catalyst for the hydrogenation reaction of methoxy-1-indanone and its application. Background technique [0002] Donepezil hydrochloride is an acetylcholinesterase inhibitor (AchEI) developed by Japan's Eisai Pharmaceutical Company, and its synthetic route is shown in Figure 1. The product was approved by the FDA in November 1996, first launched in the United States in January 1997, and launched in China in October 1999. This product is highly selective for neuronal acetylcholinesterase, has no liver toxicity, and is clinically used for the treatment of Alzheimer's disease. 2-(1-benzyl-4-piperidine methylene)-5,6-dimethoxy-1-indanone (I) is the key intermediate of donepezil hydrochloride, which can be obtained by hydrogenation and salt for...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/755B01J23/89B01J23/80B01J23/745B01J23/72B01J23/75B01J23/06C07D211/32
Inventor 牛志刚赵继全张月成叶家峰于树岭
Owner CANGZHOU SENARY CHEM SCI TEC
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