反応 #155373

ord-02c12e876b0d4c54872a87cf3dfdf4d9

反応方程式

[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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  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
    その他The product was isolated by filtration
  6. 6
    その他used without further purification

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08821871B2uspto-grants-2014_09