反応 #1994320

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

S-octyl chlorothioformate

→

title compound

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

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 9:1)

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 (0.300 g, 0.64 mmol) in dichloromethane (3.0 mL) was added triethylamine (90 μL, 0.65 mmol), then S-octyl chlorothioformate (0.133 g, 0.64 mmol). The resulting homogeneous reaction mixture was stirred for 0.5 h at 20° C. The reaction mixture was then concentrated in vacuo and the residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 9:1) affording the title compound as yellow crystals with a melting point of 98-102° C.

出典