반응 #155373

ord-02c12e876b0d4c54872a87cf3dfdf4d9

반응 방정식

[Na+].[OH-]
sodium hydroxide
CCOC(=O)CCN(C(=O)c1ccc2c(c1)nc(CNc1ccc(C#N)cc1)n2C)c1ccccn1
3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-pyridin-2-yl-amino)-propionic acid ethyl ester
Cn1c(CNc2ccc(C#N)cc2)nc2cc(C(=O)N(CCC(=O)O)c3ccccn3)ccc21
3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-pyridin-2-yl-amino)-propionic acid

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONca. 350 mL ethanol were distilled off
  2. 2
    workup.ADDITIONca. 100 mL water was added
  3. 3
    workup.ADDITIONThen diethylether (50 mL) was added
  4. 4
    workup.STIRRINGthe mixture stirred over night
  5. 5
    기타The product was isolated by filtration
  6. 6
    기타used without further purification

실험 절차

To a solution of sodium hydroxide (50.0 mmol) in 500 mL ethanol and 50 mL water was added 3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-pyridin-2-yl-amino)-propionic acid ethyl ester (41.4 mmol). The mixture was stirred at room temperature for three hours, then ca. 350 mL ethanol were distilled off, ca. 100 mL water was added and the pH was adjusted to 6. Then diethylether (50 mL) was added and the mixture stirred over night. The product was isolated by filtration and used without further purification.

출처

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