Method for synthesizing 4-pyrazinyl pyrimidine-2-sodium sulfonate

Method for synthesizing 4-pyrazinyl pyrimidine-2-sodium sulfonate

  • CN 105,153,123 A
  • Filed: 09/29/2015
  • Published: 12/16/2015
  • Est. Priority Date: 09/29/2015
  • Status: Active Application
First Claim
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1. a synthetic method for 4-pyrazinyl pyrimidine-2-sodium sulfonate, is characterized in that comprising the steps:

  • The synthesis of step one, 3-(dimethylamino)-1-(2-pyrazinyl)-2-propylene-1-ketoneTake 32.67g acetylpyrazine in the dry 500ml round-bottomed flask being placed with magneton, add 50mlDMF, then add 35.8mlN, dinethylformamide dimethylacetal, finally adds 100mlDMF;

    By added raw material round-bottomed flask in oil bath pan with 110 DEG C of backflow 6h, then be cooled to 80 DEG C of direct underpressure distillation, after steaming about 100ml liquid, stop distillation, now in mixed phase, liquid is black;

    Black liquor in flask is cooled to room temperature, now has a large amount of yellow solid to separate out, in flask, add the dispersion of 250ml anhydrous diethyl ether, flask is placed on refrigerator and cooled and freezes and spend the night, crystallization, suction filtration, washs solid with anhydrous diethyl ether, obtains greenish yellow solid;

    The synthesis of step 2,4-pyrazinyl pyrimidine thiophenolTake 5g sodium, add after chopping in batches and fill in the 1000ml round-bottomed flask of 500ml dehydrated alcohol, after solid sodium dissolves completely, add 45.21g3-(dimethylamino)-1-(2-pyrazinyl)-2-propylene-1-ketone and 19.41g thiocarbamide, backflow 10h, separates out without solid;

    Cooling, regulates pH with HAC, and limit adjusting edge stirs, and starts without obvious phenomenon, then has a large amount of solid to separate out, frozen by flask and spend the night, suction filtration in refrigerator and cooled, with absolute ethanol washing, dry must solid product;

    The synthesis of step 3,4-pyrazinyl pyrimidine-2-sodium sulfonateTake 19g4-pyrazinyl pyrimidine thiophenol in the clean 500ml round-bottomed flask putting into magneton, measure 400ml deionized water with graduated cylinder, take 4gNaOH, NaOH deionized water batch dissolution is added in flask, shake all;

    Treat all to dissolve and be placed on magnetic agitation instrument by oil bath pan 60 DEG C of heated and stirred;

    Measuring 100ml hydrogen peroxide is placed in constant voltage separating funnel, and slowly in instillation flask, in flask, color shoals gradually;

    Be added dropwise to complete rear reaction 4h, take out flask, now have solid to separate out in flask, and solution is light yellow, suction filtration obtains solid A, filtrate is placed in underpressure distillation on Rotary Evaporators, adds NaOH solution and make system be alkalescence after boiling off large quantity of fluid;

    Liquid after suction filtration is added acetone and is placed in freeze overnight in refrigerator, take out sample, suction filtration obtains solid B, blended solid A and B, i.e. 4-pyrazinyl pyrimidine-2-sodium sulfonate.

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