反应详情

A solution of 20 parts of sodium hydroxide and 300 parts of water is cooled to ±10° C. and there are added successively 41.8 parts of carbon disulfide and then dropwise 95 parts of 1-phenyl-cyclopentylmethylamine (exothermic reaction). Upon completion, the cooling-bath is removed and the whole is stirred at 30 minutes at room temperature. Then there are added dropwise at 30° C., 54.25 parts of ethyl chloroformate (exothermic reaction: cooling is necessary). The whole is stirred for 3 hours at 50° C. The reaction mixture is cooled and the product is extracted with benzene. The extract is dried, filtered and evaporated. The oily residue is distilled, yielding 86 parts of (1-phenylcyclopentylmethyl)isothiocyanate; bp. 125° C. at 0.2 mm pressure; nD20 :1.5848; d2020 :1.0910.

1. customto ±10° C.
2. customUpon completion, the cooling-bath is removed
3. additionThen there are added dropwise at 30° C.
4. stirringThe whole is stirred for 3 hours at 50° C
5. temperatureThe reaction mixture is cooled
6. extractionthe product is extracted with benzene
7. customThe extract is dried
8. filtrationfiltered
9. customevaporated
10. distillationThe oily residue is distilled