反応 #1994326

反応方程式

6-{[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carbonyl]-amino}-5-methyl-2H-indazole-7-carboxylic acid isopropyl amide

(chlorocarbonylthio)-acetic acid ethyl ester

triethylamine

→

desired compound

(6-{[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carbonyl]-amino}-7-isopropylcarbamoyl-5-methyl-indazole-2-carbonylsulfanyl)-acetic acid ethyl ester

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated
2. 2
   その他the residue was purified by flash chromatography over silica gel using a 50% ethyl acetate-50% cyclohexane mixture

実験手順

In a vial, 6-{[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carbonyl]-amino}-5-methyl-2H-indazole-7-carboxylic acid isopropyl amide (0.200 g, 0.427 mmol) was suspended in chloroform (1 ml), then a solution of (chlorocarbonylthio)-acetic acid ethyl ester (0.086 g, 0.471 mmol) in chloroform (1 ml) was added, followed by triethylamine (0.065 ml). The reaction mixture became a clear solution that was stirred for 1 hour at a temperature of 20° C. The reaction mixture was concentrated and the residue was purified by flash chromatography over silica gel using a 50% ethyl acetate-50% cyclohexane mixture. The desired compound was isolated as a yellow solid showing the physical properties reported in the corresponding table (P.41.).

出典