[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][OH:11])[C:5]([NH2:12])=[C:4]([Cl:13])[N:3]=1.[C:14]([O-])([O-])=[O:15].[K+].[K+].ClC(OC1C=CC([N+]([O-])=O)=CC=1)=O>C(#N)C>[NH2:1][C:2]1[N:7]=[C:6]2[C:5]([NH:12][C:14](=[O:15])[N:8]2[CH2:9][CH2:10][OH:11])=[C:4]([Cl:13])[N:3]=1A mixture of 2-[(2,5-diamino-6-chloro-pyrimidin-4-yl)amino]ethanol obtained in step 1 (10.0 g, 49.26 mmol) in acetonitrile (400 ml) were cooled to 0° C. To this reaction mixture K2CO3 (20.39 gm, 147.7 mmol) and 4-nitrophenyl chloroformate (19.8 g, 98.52 mmol)was added and stirred at 25-27° C. for 24 hours. This reaction mixture was filtered and washed with acetonitrile (300 ml) and diethyl ether (300 ml) respectively. Solid obtained was dried to obtain crude 2-amino-6-chloro-9-(2-hydroxyethyl)-7H-purin-8-one as a yellow solid. Small amount of crude material was purified by column chromatography to obtain pure product.
Loading…
