反应详情

温度

-15 °C

49.9 g (0.18 mol) of 2-mercaptobenzoic acid N-(3,5,5-trimethyl-cyclohexyl)-amide are initially introduced into 200 ml of tetrahydrofuran. The solution is cooled to -15° C. and 33.3 g (0.54 mol) of cyanogen chloride, dissolved in 50 ml of tetrahydrofuran, are added dropwise in the course of 30 minutes such that the internal temperature does not exceed -5° C. When the dropwise addition has ended, the mixture is allowed to come to room temperature in the course of 1 hour and stirring is then continued at this temperature for a further 2 hours. Excess cyanogen chloride and some of the solvent are distilled off under reduced pressure. The solution is poured into water, with vigorous stirring, and the solid which has precipitated is filtered off with suction and dried in a desiccator. 47 g (86.5% of theory) of 2-thiocyanato-benzoic acid N-(3,5,5-trimethylcyclohexyl)-amide are obtained as a colorless powder of melting point 117° C.

1. additionare added dropwise in the course of 30 minutes such that the internal temperature
2. customdoes not exceed -5° C
3. additionWhen the dropwise addition
4. customto come to room temperature in the course of 1 hour
5. distillationExcess cyanogen chloride and some of the solvent are distilled off under reduced pressure
6. additionThe solution is poured into water, with vigorous stirring
7. customthe solid which has precipitated
8. filtrationis filtered off with suction
9. customdried in a desiccator