四巯基苯

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 3-1 sulfonating flask, 1,850 ml of dry n-propylamine and 9.6 g of granulated lithium are initially introduced under a nitrogen inert atmosphere. The mixture is stirred at room temperature until the blue colour persists, and 55.0 g of solid 1,2,4,5-tetraethylthiobenzene are then added. A slight exothermic reaction sets in, which is kept under control by cooling with an ice-bath to prevent the inside temperature of pg,7 the solution from exceeding 38° C. After the exothermic reaction has subsided, stirring is continued for 16-20 hours under a gentle stream of N2, a further 400 mg of lithium are then added, and the mixture is heated at the reflux temperature for half an hour. The mixture is then cooled to 10° C. and 18.5 g of dry NH4Cl are added in portions. The mixture is heated to the boiling temperature of propylamine, about 1,500 ml of which are distilled off. The suspension, which has become viscous and greenish, is cooled to 5° C. and brought to a pH of 1 by the dropwise addition of 5N HCl. The temperature should not exceed 10° C. during this addition. The 1,2,4,5-tetramercaptobenzene which precipitates during the acidification is extracted from the reaction mixture with 1 times 1 liter and 2 times 500 ml of chloroform under an inert gas, the organic phase is dried with Na2SO4 and then evaporated to half its volume and cooled to -21° C. Tetramercaptobenzene precipitates as slightly greenish crystals. Yield: 20.5 g (57.5% of theory). Melting point (m.p.): 139°-142° C. are then added A slight exothermic reaction sets in, which by cooling with an ice-bath from exceeding 38° C After the exothermic reaction the mixture is heated at the reflux temperature for half an hour are distilled off greenish, is cooled to 5° C. brought to a pH of 1 by the dropwise addition of 5N HCl The temperature should not exceed 10° C. during this addition The 1,2,4,5-tetramercaptobenzene which precipitates during the acidification is extracted from the reaction mixture with 1 times 1 liter and 2 times 500 ml of chloroform under an inert gas the organic phase is dried with Na2SO4 evaporated to half its volume cooled to -21° C Tetramercaptobenzene precipitates as slightly greenish crystals 139°-142° C.