반응 #155372

ord-8f6931dbce994389892705f0d0639f67

반응 방정식

Cn1c(CNc2ccc(C#N)cc2)nc2cc(C(=O)N(CCC(=O)NCCCCNC(=O)OC(C)(C)C)c3ccccc3)ccc21
1f
Cn1c(CNc2ccc(C#N)cc2)nc2cc(C(=O)N(CCC(=O)NCCCCNC(=O)OC(C)(C)C)c3ccccc3)ccc21
{4-[3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-phenyl-amino)-propionylamino]-butyl}-carbamic acid tert-butyl ester
O=C([O-])[O-].[NH4+].[NH4+]
ammonium carbonate
Cn1c(CNc2ccc(C(=N)N)cc2)nc2cc(C(=O)N(CCC(=O)NCCCCN)c3ccccc3)ccc21
2-[(4-Carbamimidoyl-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carboxylic acid[2-(4-amino-butylcarbamoyl)-ethyl]-phenyl-amide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타evaporated to dryness at 30° C
  2. 2
    workup.DISSOLUTIONThe remaining raw material was dissolved in 200 mL dry ethanol
  3. 3
    workup.STIRRINGthe mixture stirred at room temperature over night
  4. 4
    기타After evaporation of the solvent the remaining raw material
  5. 5
    기타was triturated with ca. 5 mL ethanol
  6. 6
    기타the undissolved material separated by filtration
  7. 7
    기타the solvent evaporated at 30° C
  8. 8
    workup.DISSOLUTIONThe product was then dissolved in 30 mL water
  9. 9
    workup.STIRRINGthe solution stirred with ca. 2 g charcoal
  10. 10
    여과filtered
  11. 11
    기타evaporated to dryness

실험 절차

The product of 1f (4.81 mmol) was dissolved in a saturated solution of HCl in ethanol (250 mL), the mixture stirred at room temperature over night and then evaporated to dryness at 30° C. The remaining raw material was dissolved in 200 mL dry ethanol, then ammonium carbonate (48.1 mmol) was added and the mixture stirred at room temperature over night. After evaporation of the solvent the remaining raw material was triturated with ca. 5 mL ethanol, the undissolved material separated by filtration and the solvent evaporated at 30° C. The product was then dissolved in 30 mL water, the solution stirred with ca. 2 g charcoal, filtered and evaporated to dryness.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08821871B2uspto-grants-2014_09