反应详情

The operation is carried out as in Stage 3 of Example 5 starting from 330 mg of trans-1,4-diaminocyclohexane and 137 mg of the product obtained in Stage 1 above, the reaction medium is taken to a temperature of approximately 140 to 145° C. for approximately 6 hours then left to return to ambient temperature and left overnight. After purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2 salification is carried out with 1.4 N hydrochloric acid in ethanol, followed by separating, washing and drying at a temperature of approximately 50° C. In this way 74 mg of expected product is obtained in the form of brown-pink crystals.

1. waitthen left
2. customto return to ambient temperature
3. waitleft overnight
4. customAfter purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2 salification
5. customby separating
6. washwashing
7. customdrying at a temperature of approximately 50° C