1-Chloro-2-nitrobenzene → 1-Chloro-2-nitrobenzene

関与物質

反応条件

反応手順

2500 parts of molten 1-chloro-2-nitrobenzene are charged to a stirred reactor and 150 parts of castor oil ethoxylate (about 15 moles of ethylene oxide per 1 mole of ricinoleic acid) and 1300 parts of water are added. The batch is heated to 60° C. and emulsified by efficient stirring. The freshly prepared sodium disulfide solution is then introduced beneath the surface of the emulsion. A total amount of 2520 parts of disulfide solution is added, the rate of addition being initially about 300 parts per hour and, towards the end of the reaction, about 100 parts per hour. The ensuing reaction is slightly exothermic and by cooling the temperature is kept in a range of 60° to 65° C.. Aggregates of 2,2'-dinitrodiphenyl disulfide and 1-chloro-2-nitrobenzene formed during the reaction are comminuted with e.g. a dismembrator. Chloronitrobenzene and resultant disulfide are continuously dispersed in the reaction medium by vigorously stirring the reaction mixture. After the total amount of disulfide solution is present in the reaction vessel, stirring is continued until the reaction mass consists of individual yellow crystals and of colourless to tea-coloured mother liquor. The batch is then cooled to 40° C., and the product is isolated by filtration and washed with cold water until the washings are colourless, affording 2897 parts of 80% 2,2'-dinitrodiphenyl disulfide, corresponding to a yield of 95% of theory. Melting point: 182°-184° C. (lit.: 196° C.).

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