Supercritical thioanisole synthesis method by using chloromethane

• Main Authors: LIAO ZUTAI, TAO MING, FAN BIN, CHEN YULIANG
• Format: Patent
• Language: Chinese; English
• Published: 22.02.2017
• Subjects: ACYCLIC OR CARBOCYCLIC COMPOUNDS; CHEMISTRY; CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION ORPROCESSING OF GOODS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; METALLURGY; ORGANIC CHEMISTRY; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS; TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINSTCLIMATE CHANGE

The invention relates to a method of synthesizing thioanisole by using chloromethane as a methylating reagent, in particular to a method comprising the following steps that thiophenol sodium and chloromethane are used as raw materials; in a high-pressure reaction vessel, the chloromethane takes a contact reaction with the thiophenol sodium in a supercritical state, wherein the mol ratio of the thiophenol sodium to the chloromethane is 1:1 to 1:10, the reaction temperature is 145 DEG C to 300 DEG C, the reaction pressure is 6.7 to 25 MPa, and the reaction time is 1 to 15 hours; after the reaction is completed, water is used for washing a reaction mixture; an oil phase is collected; reduced pressure distillation is performed; fraction (10mmHg, 67 to 69 DEG C) is collected. 本发明涉及采用氯甲烷作为甲基化试剂合成茴香硫醚的方法，具体涉及以苯硫酚钠、氯甲烷为原料，在高压反应器中，使氯甲烷在超临界状态下与苯硫酚钠接触反应，苯硫酚钠与氯甲烷的摩尔比为1∶1～1∶10，反应温度为145℃～300℃，反应压力为6.7～25MPa，反应时间为1～15小时。在反应结束后，用水洗涤反应混合物，收集油相，减压精馏，收集(10mmHg，67-69℃)馏分。