Triethylamine → 6-Benzyloxyamino-4-chloro-2,5-diformamidopyrimidine

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Reaktionsschritte

A mixture of 4,6-dichloro-2,5-diformamido-pyrimidine (1.9g, 8.09mmol), benzyloxyamine (1g, 8.13mmol), triethylamine (2ml) and dioxan (20ml) was stirred at 100° C. for 1 hour. The cooled reaction mixture was filtered and the precipitate collected and washed with dioxan (2×5ml). The filtrate and washings were combined and evaporated to a syrup. Column chromatography on silica gel (eluted with chloroform-ethanol, 30:1) afforded the title compound (1.2g, 46%). IR: υmax (KBr) 3242, 1694, 1588, 1472cm-1 ; 1H NMR δH [(CD3)2SO], 4.89 (2H, s, OCH2Ph), 7.4 (5H, m, Ph), 8.15 (1H, s, CHO), 9.18, 9.42 (1H, 2×br.s, D2O exchangeable, NH), 9.25 (1H, br.s, CHO), 10.91 (2H, br.s, D2O exchangeable, 2×NH). m/e (FAB +ve ion, thioglycerol) MH+ 322.

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