HCID 21923081, compound → HCID 178478744, compound

Participants

Reaction Steps

The operation is carried out as in Stage 2 of Example 10 starting from 292 mg of the product obtained in Stage 1 above and 810 mg of trans-1,4-diaminocyclohexane and the reaction medium is heated to approximately 140° C. for approximately 3 hours then returned to 80° C., 5 ml of AtOEt then 10 ml of warm water are added, followed by leaving to return to ambient temperature, extracting with 2×10 ml of ethyl acetate, washing with 10 ml of saturated sodium chloride and 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 167 mg of expected product is obtained in the form of white solid.

Provenance & Evidence