Hydrochloric Acid → HCID 178528017, compound

Participants

Reaction Steps

A solution of 12.2 g of trans-4-(4-aminocyclohexyl)-butylcyclohexane in 135 ml of dichloromethane is added dropwise at 0° under nitrogen to a solution of 15.2 g of 1,1'-thiocarbonyldiimidazole in 90 ml of dichloromethane in the course of 1.5 hours. After standing overnight, about 140 ml of 3% hydrochloric acid are added at 0°-4° until pH 2 is obtained. The organic phase separated off is washed with water until pH 6, is dried over sodium sulfate and evaporated. Purification of the crude product (15.6 g) by column chromatography leaves 13.1 g of trans-4-(4-isothiocyanatocyclohexyl)-butylcyclohexane. Melting point (m.p.) +23°; clear point (c.p.) +72.9°.

Provenance & Evidence