Ethyl Acetate → HCID 178479704, compound

Participants

Reaction Steps

1 g of trans-1,4-aminocyclohexanol is mixed which is then taken to a temperature of 50 to 60° C. and 212 mg of the product obtained in Stage 1 above is added and taken to a temperature of 140 to 150° C. for approximately 4 hours. The reaction medium is then left to return to a temperature of 100° C., 10 ml of water is added, the reaction medium is left to settle, 10 ml of water, 20 ml of ethyl acetate are added and the medium is taken to a temperature of approximately 70° C. Then 10 ml of water is added and the reaction medium is left overnight at ambient temperature, then left to settle, followed by re-extracting with 2×20 ml of methylene chloride with 20% of methanol, combining the organic phases, washing with 10 ml of water and 10 ml of an aqueous solution of sodium chloride, drying and evaporating to dryness. The residue is then dissolved in the minimum amount of ethanol, 1.4N hydrochloric acid in ethanol is added and the reaction medium is left to crystallize, followed by diluting in 5 ml of ethanol then leaving for one hour at ambient temperature, separating, washing with 10 ml of ethanol and drying at a temperature of approximately 50° C. In this way 215 mg of expected product is obtained in the form of white crystals.

Provenance & Evidence