Reaktion #2161252

ord-3e6e0f1c13404d6da8fbdd0982d91a52

Reaktionsgleichung

CCOC(=O)c1nc(NC(=O)Nc2ccc(Cl)cc2C)cn1CC1CC1
ethyl 4-({[(4-chloro-2-methylphenyl)amino]carbonyl}amino)-1-(cyclopropylmethyl)-1H-imidazole-2-carboxylate
O
water
[Na+].[OH-]
sodium hydroxide
Cc1cc(Cl)ccc1NC(=O)Nc1cn(CC2CC2)c(C(=O)O)n1
4-({[(4-Chloro-2-methylphenyl)amino]carbonyl}amino)-1-(cyclopropylmethyl)-1H-imidazole-2-carboxylic acid

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated in vacuo
  2. 2
    workup.ADDITION100 ml of 1N hydrochloric acid are added with ice cooling
  3. 3
    FiltrationThe crystals are collected by suction filtration
  4. 4
    Sonstigedried at 40° C. in vacuo

Vorschrift

10.6 g (28.1 mmol) of ethyl 4-({[(4-chloro-2-methylphenyl)amino]carbonyl}amino)-1-(cyclopropylmethyl)-1H-imidazole-2-carboxylate are suspended in 158 ml of ethanol. With ice cooling, 16.4 ml of water and 6 ml (112 mmol) of a 50% aqueous sodium hydroxide solution are added. The reaction mixture is stirred at room temperature for 1 h and then concentrated in vacuo. The residue is taken up in 100 ml of isopropanol, and 100 ml of 1N hydrochloric acid are added with ice cooling. The crystals are collected by suction filtration and dried at 40° C. in vacuo.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07919489B2uspto-grants-2011_04