反応 #2330546

反応方程式

triethylamine

9H-fluoren-9-one-4-carboxylic acid chloride

4-fluoro-5-(4-methylpiperazin-1-yl)benzene-1,2-diamine

→

diisopropyl ether

[2-amino-4-fluoro -5-(4-methyl piperazin-1-yl)phenyl]amide

収率 74.7%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他can be prepared
2. 2
   その他After purification by flash chromatography on silica gel (40-63 μm)
3. 3
   洗浄eluting with a mixture of dichloromethane and methanol (95/5 by volume)

実験手順

The procedure used in stage 1 of Example 1 is followed, but starting from 2.69 g of 4-fluoro-5-(4-methylpiperazin-1-yl)benzene-1,2-diamine, which can be prepared according to J. Het. Chem. 2005, 42(1), 67-71, 2.82 ml of triethylamine and 2.43 g of 9H-fluoren-9-one-4-carboxylic acid chloride in 50 ml of dichloromethane for 20 hours at room temperature. After purification by flash chromatography on silica gel (40-63 μm), eluting with a mixture of dichloromethane and methanol (95/5 by volume), and then formation of a paste with diisopropyl ether, in this way we obtain 1 g of [2-amino-4-fluoro -5-(4-methyl piperazin-1-yl)phenyl]amide of 9-oxo-9H-fluorene-4-carboxylic acid, in the form of an orange powder, which is used as it is in the following stage, with the following characteristics:

出典