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公开(公告)号:US5367082A
公开(公告)日:1994-11-22
申请号:US11767
申请日:1993-02-01
Applicant: Manfred J. Bergfeld , Norbert Gutlein , Klaus Wohlfahrt , Eberhard Aust
Inventor: Manfred J. Bergfeld , Norbert Gutlein , Klaus Wohlfahrt , Eberhard Aust
IPC: C07D277/72
CPC classification number: C07D277/72 , Y02P20/582
Abstract: In a process for the preparation of 2-mercaptobenzothiazole from aniline, sulfur and carbon disulfide under pressure and for separation of the 2-mercaptobenzothiazole from the crude reaction product by cooling and recycling the desirable intermediates and by-products into the reactor together with aniline, sulfur and carbon disulfide, the reaction is carried out using a residence time in the reactor of at least one hour to a time before the 2-mercaptobenzothiazole product thus-formed begins to decompose into undesirable intermediate products. A maximum hydrogen sulfide pressure is maintained on quenching to a temperature ranging between 220 and 280.degree. C. by mixing the crude reaction product with carbon disulfide at a temperature sufficient to obtain a homogeneous quenched mixture. The hydrogen sulfide is removed completely only after crystallization of the 2-mercaptobenzothiazole.
Abstract translation: 在压力下从苯胺,硫和二硫化碳制备2-巯基苯并噻唑的方法中,通过与苯胺一起冷却和再循环所需的中间体和副产物,将2-巯基苯并噻唑与粗反应产物分离, 硫和二硫化碳,反应在反应器中停留时间至少1小时至此后由此形成的2-巯基苯并噻唑产物开始分解成不期望的中间产物。 通过在足以获得均匀淬火的混合物的温度下将粗反应产物与二硫化碳混合,将淬火后的最大硫化氢压力维持在220-280℃的温度。 仅在2-巯基苯并噻唑结晶后才完全除去硫化氢。