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Leuprolide acetate preparing method

A technology of leuprolide acetate and leuprolide, applied in peptide preparation methods, chemical instruments and methods, organic chemistry, etc., can solve problems such as complex production procedures, difficulty in salt conversion, long cycle, etc., and increase time and workload, increase product yield, and reduce the effect of waste liquid discharge

Inactive Publication Date: 2016-06-01
GL BIOCHEM SHANGHAI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It mainly solves technical problems such as complex production process, long cycle, high cost, low yield and difficulty in salt conversion in the existing leuprorelin acetate purification preparation method

Method used

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  • Leuprolide acetate preparing method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: refer to figure 1

[0029] 1. Synthesis of crude leuprolide: solid phase resin Boc-Pro- ( polystyrene resin) placed in the reaction flask, with anhydrous CH 2 Cl 2 Wash 3 times, stir for 10 minutes each time, and drain. Deprotection group: add 9-10NHCl / iPrOH+CH 2 Cl 2 , stirred for 60 minutes, and drained. Washing: CH 2 Cl 2 Wash 3 times and drain; DMF wash 1 time and drain. Neutralization: adding triethylamine / CH 2 Cl 2 Wash 3 times, stir for 5 minutes each time, and drain. Washing: Wash once with DMF and drain; CH 2 Cl 2 Wash 5-6 times until neutral, then drain. Dipeptide connection: Boc-Arg·HClHOBT and DCCI were respectively dissolved in anhydrous DMF and poured into the resin, the mouth of the bottle was tightly sealed, and stirred overnight. The next day, the solvent was drained and washed with CH 2 Cl 2 Wash 3 times, wash 4 times with absolute ethanol, wash 2 times with DMF, CH 2 Cl 2 Wash 3 times and drain. Detection of free a...

Embodiment 2

[0042] Embodiment 2: refer to figure 1

[0043] 1. Synthesis of crude leuprolide: solid phase resin Boc-Pro- ( polystyrene resin) placed in the reaction flask, with anhydrous CH 2 Cl 2 Wash 3 times, stir for 10 minutes each time, and drain. Deprotection group: add 9-10NHCl / iPrOH+CH 2 Cl 2 , stirred for 60 minutes, and drained. Washing: CH 2 Cl 2 Wash 3 times and drain; DMF wash 1 time and drain. Neutralization: adding triethylamine / CH 2 Cl 2 Wash 3 times, stir for 5 minutes each time, and drain. Washing: Wash once with DMF and drain; CH 2 Cl 2 Wash 5-6 times until neutral, then drain. Dipeptide connection: Boc-Arg·HClHOBT and DCCI were respectively dissolved in anhydrous DMF and poured into the resin, the mouth of the bottle was tightly sealed, and stirred overnight. The next day, the solvent was drained and washed with CH 2 Cl 2 Wash 3 times, wash 4 times with absolute ethanol, wash 2 times with DMF, CH 2 Cl 2 Wash 3 times and drain. Detection of free a...

Embodiment 3

[0056] Embodiment 3: refer to figure 1

[0057] 1. Synthesis of crude leuprolide: solid phase resin Boc-Pro- ( polystyrene resin) placed in the reaction flask, with anhydrous CH 2 Cl 2 Wash 3 times, stir for 10 minutes each time, and drain. Deprotection group: add 9-10NHCl / iPrOH+CH 2 Cl 2 , stirred for 60 minutes, and drained. Washing: CH 2 Cl 2 Wash 3 times and drain; DMF wash 1 time and drain. Neutralization: adding triethylamine / CH 2 Cl 2 Wash 3 times, stir for 5 minutes each time, and drain. Washing: Wash once with DMF and drain; CH 2 Cl 2 Wash 5-6 times until neutral, then drain. Dipeptide connection: Boc-Arg·HClHOBT and DCCI were respectively dissolved in anhydrous DMF and poured into the resin, the mouth of the bottle was tightly sealed, and stirred overnight. The next day, the solvent was drained and washed with CH 2 Cl 2 Wash 3 times, wash 4 times with absolute ethanol, wash 2 times with DMF, CH 2 Cl 2 Wash 3 times and drain. Detection of free a...

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Abstract

The invention relates to a leuprolide acetate preparing method to mainly solve the technical problems of existing leuprolide acetate preparing methods that the production process is complicated, the period is long, the cost is high, the yield is low, and salt conversion is difficult.According to the technical scheme, a leuprorelin crude product is obtained through solid-phase synthesis, the leuprorelin crude product is dissolved, filtered and detected, and then coarse purification, fine purification, concentration, salt conversion, recondensation and filtration are conducted on the leuprorelin crude product by means of an invert high liquid-phase chromatographic system, and finally freeze drying is conducted to obtain a white flocculent powdery product.The purification preparing method is suitable for laboratory research and development as well as large-scale industrial production.

Description

Technical field [0001] The invention relates to a method for preparing leuprolide acetate, which specifically utilizes reversed-phase high-performance liquid chromatography to perform isocratic and gradient elution on solid-phase synthesized crude leuprolide, and transfer it to Preparation method of salt. Background technique [0002] Prostate cancer is very common around the world. According to statistics from the World Health Organization's International Agency for Research on Cancer in 2012, there were 1.1 million newly diagnosed prostate cancer patients worldwide that year, accounting for approximately 15% of the total number of new cancer cases, making it the most common prostate cancer among men worldwide. The second most common cancer. The "2015 Cancer Statistics" report released by the American Cancer Society (ACS) estimates that there will be 1,658,370 new cancer cases in the United States in 2015, of which 26% of male cases will be prostate cancer, ranking first a...

Claims

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Application Information

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IPC IPC(8): C07K7/23C07K1/20C07K1/06C07K1/04
CPCC07K7/23
Inventor 张德志赵晶徐红岩
Owner GL BIOCHEM SHANGHAI
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