Water → HCID 178479703, compound

Participants

Reaction Steps

575 mg of trans-1,4-aminocyclohexanol are mixed together and the reaction medium is taken to a temperature of 50 to 60° C. then 313 mg of the product obtained in Stage 1 above is added and agitation is carried out at a temperature of 150 to 160° C. for approximately 20 hours. The reaction medium is then left to return to ambient temperature, taken up in ethyl acetate and water and then taken to a temperature of approximately 60° C. and left to settle, followed by re-extracting with ethyl acetate, washing with a saturated aqueous solution of sodium chloride, drying and evaporating to dryness. The residue is chromatographed on silica (eluent: CH2Cl2/MeOH 95/5), taken up in an ethanolic solution of hydrochloric acid and left to crystallize, followed by separating, drying under reduced pressure and 266 mg of expected product is recovered.

Provenance & Evidence