Hydrochloric Acid → HCID 178447931, compound

Participants

Reaction Steps

20.3 g of benzenesulphonyl chloride are added while stirring to a mixture of 9.45 g of trans-2-(4-propylcyclohexyl)-5-pyrimidinecarboxamide and 55 ml of pyridine. After 2 hours, the solution is poured into a mixture of 100 g of ice and 0.9 ml of half-concentrated hydrochloric acid. The precipitated product is taken up in ether and the ether extract is washed neutral with water, dried and evaporated. The crude product is purified by chromatography on 200 g of silica gel with hexane/benzene (1:1) and subsequent bulb-tube distillation at 135° C./0.05 mmHg. There is obtained trans-2-(4-propylcyclohexyl)-5-pyrimidinecarbonitrile; m.p. 74° C., cl.p 89.5° C., smectic-nematic phase transition 71.5° C. (monotropic).

Provenance & Evidence