反应详情

温度

20 °C

To a reactor fitted with a stirrer, condenser and addition funnel was charged 20 parts of mercaptobenzothiazole (MBT) and 160 parts of methanol. The mixture was heated and refluxed at atmospheric pressure until the MBT dissolved. To the solution was then mixed, by adding dropwise, 46.8 parts of a methanol solution of 30 weight percent hydrogen peroxide which had been prepared by dissolving 6.8 parts of 30 weight percent hydrogen peroxide in 40 parts methanol while stirring the mixture at reflux. After the addition, the resultant mixture was stirred for an additional 20 minutes. The mixture was then allowed to cool to about 20° C. and was filtered. The dibenzothiazolyl disulfide produced was dried under vacuum at 40° C. and its melting point determined to be 180° C. The melting point was determined with a capillary tube with a heating rate of 1° C. per minute. In the conduct of the reaction, only water was formed as a byproduct instead of the typical organic impurity precipitates mixed with the disulfide which typically occur during the oxidation of the sodium salt of the mercaptobenzothiazole in an aqueous solution.

1. customTo a reactor fitted with a stirrer, condenser and addition funnel
2. temperatureThe mixture was heated
3. dissolutiondissolved
4. additionTo the solution was then mixed
5. additionby adding dropwise
6. temperatureat reflux
7. additionAfter the addition
8. filtrationwas filtered