반응 #3497

ord-a24726e74e5d4a6ca7abb5ec691259ae

반응 방정식

O=C(Nc1ccc([N+](=O)[O-])cc1)N(C[C@H]1CC[C@H](CN(C(=O)Nc2ccc([N+](=O)[O-])cc2)C2CCCCC2)CC1)C1CCCCC1
trans-1,4-bis[[1-cyclohexyl-3-(4-nitrophenyl)ureido]-metyl]cyclohexane
[H][H]
Hydrogen
Nc1ccc(NC(=O)N(C[C@H]2CC[C@H](CN(C(=O)Nc3ccc(N)cc3)C3CCCCC3)CC2)C2CCCCC2)cc1
white crystals
수율 106.6%
Nc1ccc(NC(=O)N(C[C@H]2CC[C@H](CN(C(=O)Nc3ccc(N)cc3)C3CCCCC3)CC2)C2CCCCC2)cc1
Trans-1,4-bis[[1-cyclohexyl-3-(4-aminophenyl)ureido]methyl]cyclohexane
수율 106.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타synthesized in accordance with Example 2
  2. 2
    기타was separated by filtration
  3. 3
    농축the reaction mixture was concentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONThe reaction mixture was dissolved in chloroform
  5. 5
    workup.ADDITIONa 4N hydrochloric acid-dioxyane solution was added

실험 절차

A 0.6 g quantity of 10% palladium carbon was added to 100 ml of a DMF solution containing 5.7 g of trans-1,4-bis[[1-cyclohexyl-3-(4-nitrophenyl)ureido]-metyl]cyclohexane synthesized in accordance with Example 2. Hydrogen was added at ordinal pressure and normal temperature for 15 hours. After completion of the reaction, palladium was separated by filtration and the reaction mixture was concentrated under reduced pressure. The reaction mixture was dissolved in chloroform and a 4N hydrochloric acid-dioxyane solution was added to provide 5.5 g (95%) of white crystals precipitated.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733931uspto-grants-1998_03