반응 #10015

반응 방정식

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

caesium carbonate

isopropyl iodide

dioxane

→

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

용매

ethyl acetate

—

mixture

DMF

water

반응 조건

후처리

1. 1
   세척the organic phase is washed with water
2. 2
   건조dried over sodium sulfate
3. 3
   기타After removal of the solvent
4. 4
   기타the residue is chromatographed over silica gel (mobile phase: CH2Cl2:methanol=9:1)
5. 5
   기타The crystalline precipitate obtained on concentration
6. 6
   여과is filtered off
7. 7
   기타dried

실험 절차

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).

출처