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Preparation method of bazedoxifene

A technology of bazedoxifene and fixed bed, which is applied in the field of bazedoxifene preparation, can solve the problems of cumbersome filtration and recovery operations, great influence on the reaction conversion rate, long reaction time, etc., and achieve simple and easy operation of the process and simplified post-treatment Steps, reactions and high safety effects

Active Publication Date: 2021-03-30
JIANGSU LONG HEALTHCARE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When this method prepares bazedoxifene, there are long reaction time, high cost, great influence on the reaction conversion rate by the quality of the palladium / carbon catalyst, high safety risk in the high-pressure reactor, unstable quality of catalyst recovery and mechanical application, and cumbersome filtration and recovery operation. There are also risks such as palladium / carbon catalyst spontaneous combustion

Method used

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  • Preparation method of bazedoxifene
  • Preparation method of bazedoxifene
  • Preparation method of bazedoxifene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as figure 1 In the process flow shown, the bazedoxifene intermediate solution and hydrogen are first mixed in the mixer 1, and then the mixed material enters the fixed bed reactor 2 for catalytic hydrogenation reaction, and the reaction material enters the gas-liquid separator 3 after the reaction The liquid product is separated from the remaining hydrogen, and finally the liquid product enters the refining equipment 4 for refining to obtain the bazedoxifene refined product, while the remaining hydrogen is returned to the mixer 1 through the compressor 5 for recycling.

[0035] In the fixed-bed hydrogenation reaction device, the palladium / carbon catalyst is packed, the hydrogen pressure is adjusted to be 1.0MPa, and the feed rate of the solution of the bazedoxifene intermediate is 0.4ml / min, respectively at 20°C, 30°C, The reaction was performed at 40°C, 50°C, 60°C, and 70°C, and the HPLC results of each component of the hydrogenation reaction are shown in Table 1....

Embodiment 2

[0040] Such as figure 1 In the fixed-bed hydrogenation reaction device shown in the process, the palladium / carbon catalyst is packed, the reaction temperature is controlled at 65°C, the feed rate of the bazedoxifene intermediate solution is 0.4ml / min, and the hydrogen pressure is adjusted to 0.1MPa respectively , 0.4MPa, 0.7MPa, 1.0MPa, 1.2MPa, 1.5MPa, reaction under 1.8MPa, the HPLC results of each component of its hydrogenation reaction are shown in Table 2.

[0041] The investigation result of table 2 different hydrogen pressures

[0042] hydrogen pressure bazedoxifene Bazedoxifene intermediate Hydrogenation reaction intermediate 0.1MPa 88.7％ 6.5％ 4.8％ 0.4MPa 93.4％ 3.0％ 3.6％ 0.7MPa 98.0％ 1.6％ 1.4％ 1.0MPa 98.3％ 0.5％ 1.2％ 1.2 MPa 98.3％ 0.4％ 1.3％ 1.5MPa 98.4％ 0.5％ 1.1％ 1.8MPa 98.2％ 0.4％ 1.4％

[0043] It can be seen from Table 2 that in the preparation method of the present application, the hydrogen pr...

Embodiment 3

[0045] Such as figure 1 In the fixed-bed hydrogenation reaction device shown in the process, the palladium / carbon catalyst is packed, the reaction temperature is controlled at 65°C, and the hydrogen pressure is adjusted to 1.0MPa. The feed rate of the bazedoxifene intermediate solution is 0.1ml / min, 0.2 ml / min, 0.3ml / min, 0.4ml / min, 0.5ml / min, 0.6ml / min, and 0.7ml / min were reacted, and the HPLC results of each component of the hydrogenation reaction were shown in Table 3.

[0046] The investigation result of table 3 different feeding speeds

[0047]

[0048] It can be seen from Table 3 that in the preparation method of the present application, the feed rate of the reaction materials preferably ranges from 0.1 to 0.7 ml / min.

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Abstract

The invention discloses a preparation method of bazedoxifene. The preparation method comprises the following steps: (1) reaction materials are mixed, and the reaction materials comprise a bazedoxifeneintermediate of formula I; (2) fixed bed catalytic reaction; (3) post-treatment. The preparation method has the advantages of realization of continuous reaction, fast reaction speed, repeated and continuous use of the catalyst and hydrogen, high reaction safety, no discharge of waste water and waste gas, environmental protection, saving, and easy realization of automation.

Description

technical field [0001] The invention relates to a method for preparing bazedoxifene, in particular to a method for preparing bazedoxifene capable of continuous operation. Background technique [0002] Bazedoxifene, English name Bazedoxifene, is an indole derivative, its chemical name is 1-(4-(2-(azepan-1-yl)ethoxy)benzyl)-2-( 4-hydroxyphenyl)-3-methyl-1H-indole-5-ol. Its chemical structural formula is as follows: [0003] [0004] Bazedoxifene is a third-generation selective estrogen receptor modulator originally developed by Wyeth, which was launched in Italy and Spain in April 2009 under the trade name Conbriza, and is used to treat osteoporosis in postmenopausal women. [0005] In the preparation method of bazedoxifene reported so far, there is a reaction step of one-step hydrogenation debenzylation: [0006] [0007] In the prior art, palladium / carbon is used as a catalyst, and a special hydrogenation reactor is used for batch and intermittent catalytic reaction...

Claims

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Application Information

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IPC IPC(8): C07D209/12
CPCC07D209/12
Inventor 肖雅付明伟
Owner JIANGSU LONG HEALTHCARE
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