反应详情

温度

50 °C

0.92 parts of sodium was dissolved in 80 parts of ethanol and to this was added 14.8 parts of 5-mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione, as prepared in example 11 dissolved in 200 parts ethanol. The mixture was then warmed to 50°C and a solution of 6.6 parts n-hexyl bromide in 50 parts ethanol was added dropwise. The mixture was refluxed for 5 hours, the ethanol evaporated, and the residue extracted with diethyl ether. Evaporation of the ether solution gave a crystalline residue which was crystallised from ether to give 12 parts of 5-n-hexylthio 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione, m.p. 110°.

1. customas prepared in example 11
2. temperatureThe mixture was refluxed for 5 hours
3. customthe ethanol evaporated
4. extractionthe residue extracted with diethyl ether
5. customEvaporation of the ether solution
6. customgave a crystalline residue which
7. customwas crystallised from ether