Ethyl Acetate → HCID 178492896, compound

Participants

Reaction Steps

The operation is carried out as in Stage 2 of Example 10 starting from 126 mg of the product obtained in Stage 1 above and 319 mg of trans-1,4-diaminocyclohexane and the reaction medium is heated to approximately 140° C. for approximately 3 hours, left to return to 80° C., 5 ml of AcOEt is added, 5 ml of warm water is added, the reaction medium is left to return to ambient temperature, followed by extracting with 2×5 ml of ethyl acetate, washing with 5 ml of saturated sodium chloride, then drying. After purification by chromatography on silica eluting with methylene chloride/methanol/ammonium hydroxide in a proportion of 85/15/1.5, 5 ml of 1.4N hydrochloric acid/ethanol is added, the reaction medium is left to crystallize, followed by filtering, rinsing with 5 ml of ether and drying under vacuum. In this way 95 mg of expected product is obtained in the form of a beige solid.

Provenance & Evidence