Ethyl Acetate → HCID 18457591, compound

Participants

Reaction Steps

656 mg of trans-1,4-diaminocyclohexane and 133 mg of the product obtained in Stage 2 above are mixed together and the reaction medium is taken to a temperature of 130 to 150° C. for approximately 5 hours then left overnight at ambient temperature. Then the reaction medium is taken up in 10 ml of water and 20 ml of ethyl acetate and left to settle, followed by re-extracting with 2×5 ml of ethyl acetate, washing with 10 ml of water and 10 ml of saturated aqueous solution of sodium chloride, drying and evaporating to dryness. After purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2, 1.5 ml of hydrochloric acid at 1.4 N in ethanol is added and the reaction medium is left to crystallize. After diluting with 2 ml of ethyl acetate and leaving for one hour at ambient temperature, separation is carried out, followed by washing with 5 ml of ethyl acetate and drying at a temperature of approximately 50° C. In this way 98 mg of expected product is obtained in the form of white/cream crystals.

Provenance & Evidence