Iodoethane → 2-Chloro-n-(3-chlorophenyl)-9-ethyl-9h-purin-6-amine

反応式

[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:25](I)[CH3:26]>CN(C=O)C>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:25][CH3:26])=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[N:3]=1

参加物

実験手順

676 mg (2.413 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-purine are dissolved in 10 ml of abs. DMF by means of gentle heating. 375 mg (2.713 mmol) of potassium carbonate, followed by 0.97 ml (12.01 mmol) of ethyl iodide are added at room temperature. The reaction mixture is stirred at room temperature for 2 hours. When the reaction is complete, the reaction mixture is poured onto ice/water (60 ml) and stirred for 10 minutes. The inhomogeneous mixture is extracted three times with ethyl acetate. The combined organic extracts are washed twice with water and once with saturated sodium chloride solution and dried over magnesium sulfate. After filtration, the filtrate is concentrated under reduced pressure at 35° C. and dried under an HV. The resulting crude product (crystalline oil) is purified by crystallization from diethyl ether/hexane. 2-Chloro-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine is obtained; Rf=0.55 (ethyl acetate:hexane=3:1); APCI-MS: (M+H)+=308; HPLC: tret(grad 20/1)=12.40 minutes; m.p. 127–128° C.