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Improved method for recovering fulvestrant with unqualified isomer ratio

A technology for fulvestrant and isomers, which is applied in the field of pharmaceutical preparation, can solve the problems of unqualified fulvestrant recovery isomer ratio, unindustrialization, potential safety hazards, etc., so as to reduce production costs, improve recovery, The effect of reducing the discharge of three wastes

Active Publication Date: 2018-02-16
HANGZHOU ALLSINO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the disadvantages of the existing technology, such as relatively large potential safety hazards, polluting the environment, and being unsuitable for industrialization, the present invention adopts a new technical solution, improves the existing preparation process, and provides a new ratio of recovered isomers The preparation method of the unqualified fulvestrant, the specific scheme is as follows:

Method used

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  • Improved method for recovering fulvestrant with unqualified isomer ratio
  • Improved method for recovering fulvestrant with unqualified isomer ratio
  • Improved method for recovering fulvestrant with unqualified isomer ratio

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Reduction reaction

[0022] Add 5 g of fulvestrant with an unqualified isomer ratio, 2.1 g of sodium bromide, 3.5 g of p-toluenesulfonic acid and 25 ml of acetone into a 100 ml three-necked flask, stir and react at 25°C-35°C for 1.5h, and the reaction solution gradually changes from After the clarification became viscous, the reaction was completed, filtered under reduced pressure, and the filtrate was concentrated under reduced pressure to obtain 4.6 g of light yellow oil.

[0023] (2) Oxidation reaction

[0024] Add 4.6g of the reduction product from the previous step into a 50ml three-necked flask, add 10.1ml of ethyl acetate and 2.63ml of acetic acid, slowly add 4.66ml of peracetic acid dropwise, keep the temperature below 25°C, and keep warm at 20°C after the addition The reaction was stirred at 25°C for 2 hours. After the reaction was completed, 25% aqueous solution of sodium thiosulfate was slowly added dropwise. Extract with 100ml of ethyl acetate, separa...

Embodiment 2

[0026] (1) Reduction reaction

[0027] Add 5g of fulvestrant with an unqualified isomer ratio, 3g NaI and 25ml of acetone into a 100ml three-necked flask, slowly add 25ml of 40% boron trifluoride ether solution dropwise, and stir and react at 25°C-35°C for 1.5h. After completion, add 30ml of toluene and 30ml of water, stir for 5min, stand still to separate the water layer, wash the toluene layer with 30ml of water, repeat once. The toluene layer was concentrated under reduced pressure at 50°C to obtain 4.4 g of light yellow oil.

[0028] (2) Oxidation reaction

[0029] Add 4.4g of the reduction product from the previous reaction to a 250ml three-necked flask, and add 44.5ml of tetrahydrofuran and 11.1ml of methanol; cool down to 0°C in an ice-salt water bath, add 4.3ml of peracetic acid, and the temperature does not exceed 5°C; the reaction solution is cloudy after adding , keep warm at 20°C-30°C for 20 hours; add 14.1ml of dichloromethane, wash the dichloromethane layer 4 t...

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Abstract

The invention relates to an improved method for recovering fulvestrant with an unqualified isomer ratio. A halide is adopted as a reduction catalyst for replacing reductants with potential safety hazard and environmental pollution in the prior art, so that the discharge of three wastes (waste gas, waste water and industrial residue) is reduced, the recovery rate of the fulvestrant is greatly improved, the recovery rate of the unqualified fulvestrant can reach about 70%, and thus the improved method is beneficial for industrial popularization.

Description

technical field [0001] The invention relates to the field of medicine preparation, in particular to an improved method for recovering fulvestrant with an unqualified isomer ratio. Background technique [0002] Fulvestrant (Fulvestrant), the chemical name is (7a,17b)-7-[9-(4,4,5,5,5-pentafluoropentasulfinyl)nonyl]-estra-1, 3,5-(10)-triene-3,17-diol, whose structural formula is: [0003] [0004] Fulvestrant is an intramuscular injection drug developed by AstraZeneca for the treatment of estrogen receptor-positive metastatic breast cancer in postmenopausal women whose disease is still getting worse after anti-estrogen therapy, 2002 Approved by the US Food and Drug Administration in April, it is the only anti-estrogen drug that can be widely used clinically after the failure of tamoxifen. A number of clinical studies have found that fulvestrant 250 mg dose is effective in treating advanced breast cancer. In the second-line treatment, it has good curative effect and stable ...

Claims

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Application Information

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IPC IPC(8): C07J31/00
Inventor 张志强李勇汪振华黄丰刘艳华
Owner HANGZHOU ALLSINO CHEM
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