反応 #10015

反応方程式

2-chloro-6-(4-nitro-phenyl-amino)-purine

caesium carbonate

isopropyl iodide

dioxane

→

2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine

溶媒

ethyl acetate

—

mixture

DMF

water

反応条件

後処理

1. 1
   洗浄the organic phase is washed with water
2. 2
   乾燥dried over sodium sulfate
3. 3
   その他After removal of the solvent
4. 4
   その他the residue is chromatographed over silica gel (mobile phase: CH2Cl2:methanol=9:1)
5. 5
   その他The crystalline precipitate obtained on concentration
6. 6
   ろ過is filtered off
7. 7
   その他dried

実験手順

A mixture comprising 0.87 g (3 mmol) of 2-chloro-6-(4-nitro-phenyl-amino)-purine, 0.15 g (4.5 mmol) of caesium carbonate and 1.8 ml (18 mmol) of isopropyl iodide is stirred in 22 ml of a mixture comprising dioxane:water:DMF in a ratio of 2:1:4 at 100° C. for 48 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is chromatographed over silica gel (mobile phase: CH2Cl2:methanol=9:1). The crystalline precipitate obtained on concentration is filtered off and dried. 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine is obtained; m.p.>260° C.; FAB-MS: (M+H)+=333; Rf=0.8 (CH2Cl2:methanol=9:1).

出典