反応 #588665

反応方程式

6-chloro-1H-indazol-3-ol

1-isocyanatohexane

→

6-chloro-3-hydroxyindazole-1-carboxylic acid hexylamide

溶媒

DMF

反応条件

後処理

1. 1
   濃縮concentration and purification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)

実験手順

100 mg (0.59 mmol) of 6-chloro-1H-indazol-3-ol were dissolved in 5 ml of DMF. Addition of 83 mg (0.65 mmol) of 1-isocyanatohexane was followed by stirring at room temperature for 1.5 h and at 50° C. for 1 h, concentration and purification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 17 mg (7%), M+H+: 296.14, 6-chloro-3-oxo-3H-indazole-1,2-dicarboxylic acid bishexylamide and 12 mg (5%) of 6-chloro-1-hexylcarbamoyl-1H-indazol-3-yl hexylcarbamate. It was additionally possible to isolate 6-chloro-3-hydroxyindazole-1-carboxylic acid hexylamide as compound not according to the invention.

出典