反应详情

The operation is carried out as in Stage 2 of Example 10 starting from 161 mg of the product obtained in Stage 1 above and 403 mg of trans-1,4-diaminocyclohexane and the reaction medium is heated to approximately 140° C. for approximately 3 hours 30 minutes left to return to 80° C., 5 ml of AcOEt then 5 ml of warm water are added, the reaction medium is left to return to ambient temperature, followed by extracting with 2×5 ml of ethyl acetate, washing with 5 ml of saturated sodium chloride, then 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 113 mg of expected product is obtained in the form of beige white crystals.

1. waitleft
2. customto return to 80° C.
3. waitthe reaction medium is left
4. customto return to ambient temperature
5. extractionby extracting with 2×5 ml of ethyl acetate
6. washwashing with 5 ml of saturated sodium chloride
7. customdrying
8. customAfter 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
9. additionis added
10. waitthe reaction medium is left
11. customto crystallize
12. filtrationby filtering
13. washrinsing with 5 ml of ether
14. customdrying under vacuum