反応 #2161256

ord-02e97cd3a4774f0d8d4ab9b568f8c9b6

反応方程式

CCOC(=O)c1nc(NC(=O)Nc2ccc(OC(F)(F)F)cc2)cn1C
ethyl 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylate
[Na+].[OH-]
sodium hydroxide
Cl
hydrochloric acid
Cn1cc(NC(=O)Nc2ccc(OC(F)(F)F)cc2)nc1C(=O)O
1-Methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylic acid

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The solution is extracted with dichloromethane
  2. 2
    濃縮The organic phase is concentrated in vacuo
  3. 3
    その他The residue is purified by preparative HPLC

実験手順

835 mg (2.13 mmol) of ethyl 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylate are suspended in 5 ml of ethanol and 12 ml of tetrahydrofuran. With ice cooling, 2 ml (25 mmol) of a 50% aqueous sodium hydroxide solution are added. The reaction mixture is stirred at room temperature overnight and then, with ice cooling, acidified with 1N hydrochloric acid. The solution is extracted with dichloromethane. The organic phase is concentrated in vacuo. The residue is purified by preparative HPLC.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07919489B2uspto-grants-2011_04