Synthesis method of sulfachloropyrazine sodium
A technology of sulfachlorpyrazine sodium and sulfachlorpyrazine sodium, which is applied in the field of synthesis of sulfachlorpyrazine sodium, can solve problems such as difficult removal and unsatisfactory, and achieve low price, high yield and product purity, and abundant sources of raw materials Effect
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[0020] A kind of synthetic method of sulfachlorpyrazine sodium, is characterized in that, comprises the steps:
[0021] Step S1, sequentially add 4-aminobenzene-1-sulfonyl chloride, 2-amino-6-chloropyrazine and an organic solvent into the reaction kettle, and then slowly add an acid-binding agent therein, and complete the addition within 2-4 hours. Stir at 0.8-1.3MPa, 30-50°C for 12-20 hours to obtain the first mixed solution, and adjust the reaction kettle to normal temperature and pressure;
[0022] Step S2, removing the solvent by suction filtration of the first mixed solution prepared in step S1 to obtain a crude product, then adding drinking water to the crude product, adjusting the pH value to 4.5-5.3 with hydrochloric acid, filtering and washing with water to obtain sulfachlorpyr Zinc;
[0023] Step S3, heating and dissolving the sulfachlorpyrazine produced in step S2 in sodium hydroxide solution, cooling and crystallizing, and filtering to obtain sulfachlorpyrazine so...
Embodiment 1
[0034] Embodiment 1 provides a kind of synthetic method of sulfachlorpyrazine sodium, is characterized in that, comprises the steps:
[0035] Step S1, add 4-aminobenzene-1-sulfonyl chloride, 2-amino-6-chloropyrazine and toluene to the reaction kettle in turn, and then slowly add sodium hydroxide to it, within 2 hours, at 0.8MPa After stirring for 12 hours at 30°C, the first mixed solution was obtained, and the reaction kettle was adjusted to normal temperature and pressure;
[0036] Step S2, suction-filtering the first mixed solution prepared through step S1 to remove the solvent to obtain a crude product, then adding drinking water to the crude product, adjusting the pH value to 4.5 with hydrochloric acid, filtering and washing with water to obtain sulfachlorpyrazine;
[0037] Step S3, heating and dissolving the sulfachlorpyrazine produced in step S2 in sodium hydroxide solution, cooling and crystallizing, and filtering to obtain sulfachlorpyrazine sodium.
[0038] The molar...
Embodiment 2
[0042] Embodiment 2 provides a synthetic method of sulfachlorpyrazine sodium, which is basically the same as in Example 1, except that 4-aminobenzene-1-sulfonyl chloride, 2-amino-6-chloropyrizine described in step S1 The mol ratio of oxazine, organic solvent, acid-binding agent is 1:1:7:0.9; Described acid-binding agent is sodium carbonate.
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