反応 #59796

反応方程式

[4,5-Bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazol-1-yl]-piperazin-1-yl-methanone

3-{4-[4,5-bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazole-1-carbonyl]-piperazin-1-yl}-propionitrile hydrochloride

methylisothiocyanate

→

4-[4,5-bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazole-1-carbonyl]-piperazine-1-carbothioic acid methylamide

溶媒

methylene chloride

反応条件

後処理

1. 1
   濃縮the reaction mixture was concentrated to dryness
2. 2
   その他Purification of the crude residue by flash chromatography (silica gel)
3. 3
   洗浄eluting with ethyl acetate and hexanes

実験手順

[4,5-Bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazol-1-yl]-piperazin-1-yl-methanone (279 mg, 0.47 mmol, example 8A) was dissolved in methylene chloride (3 mL) and methylisothiocyanate (64 uL) was added. After stirring 3 h, the reaction mixture was concentrated to dryness. Purification of the crude residue by flash chromatography (silica gel) eluting with ethyl acetate and hexanes gave 4-[4,5-bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazole-1-carbonyl]-piperazine-1-carbothioic acid methylamide (195 mg). LR-MS: 664.4 [(M+H)+].

出典