反应详情

400 mg of trans-1,4-diaminocyclohexane is taken to a temperature of 60 to 70° C., then 119 mg of the product obtained in Stage 2 above is added and the reaction medium is taken to a temperature of 130 to 140° C. for 3 hours, then left to return to ambient temperature, 5 ml of water is added followed by extracting with 3×10 ml of ethyl acetate, washing with 10 ml of water and 5 ml of an 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, followed by salification with 1.4N hydrochloric acid in ethanol, leaving to crystallize for 2 days at ambient temperature, separating, washing with 10 ml of ethanol and drying at a temperature of approximately 50° C. In this way 112 mg of expected product is obtained in the form of crystals white/cream.

1. customis taken to a temperature of 60 to 70° C.
2. waitleft
3. customto return to ambient temperature
4. extractionby extracting with 3×10 ml of ethyl acetate
5. washwashing with 10 ml of water and 5 ml of an aqueous solution of sodium chloride
6. customdrying
7. customevaporating to dryness
8. customAfter purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2
9. customleaving
10. customto crystallize for 2 days at ambient temperature
11. customseparating
12. washwashing with 10 ml of ethanol
13. customdrying at a temperature of approximately 50° C