反応 #1994321

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 isopropylamide

triethylamine

methanesulphonyl chloride

→

title compound

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

溶媒

dichloromethane

反応条件

後処理

1. 1
   濃縮The reaction mixture was then concentrated in vacuo
2. 2
   その他the residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1)
3. 3
   その他yielding a brown solid that
4. 4
   その他was recrystallized from ethyl acetate

実験手順

To a suspension of 6-{[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carbonyl]-amino}-5-methyl-2H-indazole-7-carboxylic acid isopropylamide (0.800 g, 1.71 mmol) in dichloromethane (5.0 mL) was added triethylamine (0.476 mL, 3.42 mmol), followed by methanesulphonyl chloride (0.265 mL, 3.42 mmol). The dark colored homogeneous reaction mixture was stirred for 1 h at 20° C. The reaction mixture was then concentrated in vacuo and the residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1) yielding a brown solid that was recrystallized from ethyl acetate to afford the title compound as colourless crystals with a melting range of 135-175° C. (with decomposition).

出典