Ethyl Acetate → HCID 178427466, compound

Participants

Reaction Conditions

Reaction Steps

320 mg of the product obtained in Stage 1 above and 844 mg of trans-1,4-diaminocyclohexane are mixed together and the reaction medium is heated to approximately 140° C. for approximately 3 hours then lowered to 80° C., 5 ml AcOEt, then 10 ml of water are added warm. The reaction medium is left to return to ambient temperature, followed by extracting with 2×10 ml of ethyl acetate, washing with 10 ml of a saturated solution of sodium chloride then drying. After purification by chromatography on silica eluting with methylene chloride/methanol/ammonium hydroxide in a proportion of 90/10/1, 1.5 ml of hydrochloric acid/ethanol 1.4N, is added followed by leaving to crystallize, filtering, rinsing with 5 ml of ether and drying under vacuum. In this way 173 mg of expected product is obtained in the form of white crystals.

Provenance & Evidence