Synthetic method of brominated alkylating agent

A synthesis method and an alkylating agent technology, applied in the field of chemical medicine, can solve the problems of low crystallization purity and unstable yield of dibromodunglitol, and achieve the effects of safe and reasonable process, easy acquisition, difficult cleaning and filtration

Active Publication Date: 2016-07-27
GUANGXI WUZHOU PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] According to the currently disclosed technical method, the obtained dibromodunglitol crystal has low purity and unstable yield; there is no public report on the corresponding refining means

Method used

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  • Synthetic method of brominated alkylating agent
  • Synthetic method of brominated alkylating agent
  • Synthetic method of brominated alkylating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (a) 10kg dulcitol is dropped into the reactor, add 40% hydrobromic acid aqueous solution: the mixed solution of formic acid=1:2 (weight ratio), add-on is 20 times of dulcitol weight;

[0068] (b) Heating to 65°C in a water bath and stirring continuously until crystallization occurs;

[0069] (c) In a closed state, under constant stirring at 65°C, add formic acid that is 5 times the weight of dulcitol, pressurize to 0.001MPa with nitrogen, continue to react for 2 hours, let cool to room temperature, and let stand for 5 hours;

[0070] (d) Dilute the reaction solution with 1 times the amount of water, filter, wash the filter cake with water until neutral, drain it, add 0.5 times the volume percentage of ethanol with a concentration of 60%, soak it for 0.1 hour, drain it, and reduce the pressure at 25°C to -0.01 Dry at mPa to obtain crude crystals of dibromodulcitol; add methanol 100 times the weight of the crude crystals to the crude crystals of dibromodulcitol, and recry...

Embodiment 2

[0073] (a) 10kg dulcitol is dropped into the reactor, add 45% hydrobromic acid aqueous solution: the mixed solution of acetic acid=1:0.001 (weight ratio), add-on is 5 times of dulcitol weight;

[0074] (b) Heating to 40°C in a water bath and stirring continuously until crystallization occurs;

[0075] (c) In a closed state, under constant stirring at 40°C, add acetic acid 20 times the weight of dulcitol, pressurize to 0.01MPa with argon, continue to react for 12 hours, let cool to room temperature, and let stand for 8 hours;

[0076] (d) Dilute the reaction solution with 2 times the amount of water, filter, wash the filter cake with water until neutral, drain it, add 1 times the volume percentage concentration of 50% ethanol to soak for 0.2 hours, drain it, and reduce the pressure to -0.02 at 30 ° C. Dry at mPa to obtain crude crystals of dibromodulcitol; add methanol 70 times the weight of the crude crystals to the crude crystals of dibromodulcitol, and recrystallize at 6°C t...

Embodiment 3

[0079] (a) 10kg dulcitol is dropped into the reactor, add 50% hydrobromic acid aqueous solution: the mixed solution of acetic acid=1:0.01 (weight ratio), add-on is 10 times of dulcitol weight;

[0080] (b) Heating to 50°C in a water bath and stirring continuously until crystallization occurs;

[0081] (c) In an airtight state and kept at 50°C under constant stirring, add acetic acid containing 33% hydrogen bromide 1 times the weight of dulcitol, feed helium to pressurize to 0.1MPa, continue to react for 18 hours, let cool to room temperature, let stand for 8 hours;

[0082] (d) Dilute the reaction solution with 3 times the amount of water, filter, wash the filter cake with water until neutral, drain it, add 5 times the volume percentage concentration of 65% ethanol to soak for 0.5 hours, drain it, and reduce the pressure at 50 ° C to -0.05 Dry at mPa to obtain crude crystals of dibromodulcitol; add methanol 80 times the weight of the crude crystals to the crude crystals of di...

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Abstract

The invention relates to a synthetic method of a brominated alkylating agent. The synthetic method of the brominated alkylating agent is used, and the product whose average yield is 50% or above and average purity is 80% or above is obtained; in a preferred range, the purity reaches 90% or above; and compared with the prior art, the effect is obviously better.

Description

technical field [0001] The invention relates to the field of chemical medicines, in particular to a synthesis method of a brominated alkylating agent. Background technique [0002] Dibromodulcitol, also known as dibromogalactitol, is an isomer of dibromomannitol, and its structure is as follows: [0003] [0004] Dibromodulcitol, also known as dibromogalactitol, is an isomer of dibromomannitol, which itself has pharmacological activity and is also the precursor of many compounds. [0005] About the synthesis of dibromodunglitol, following preparation method has been disclosed: [0006] The preparation method disclosed in the second phase of "Journal of Jiangxi Medical College" in 1984 in "The Synthesis of Anticancer Agent Dibromoguardol" is: under normal pressure, the optimum temperature for synthesizing dibromoguardol is 90 ℃ ( ±1°C) The suitable heating time is 9 hours; the concentration of hydrobromic acid should not be lower than 69-70%, otherwise the yield will be ...

Claims

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Application Information

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IPC IPC(8): C07C31/42C07C29/62C07C29/74
Inventor 赵学伟黄宇声陈勇徐卓李锦雄陈骞卢蕾羽
Owner GUANGXI WUZHOU PHARMA GRP
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