反应详情

A solution of (4-amino-5-benzyl-pyrimidin-2-ylsulfanyl)-acetic acid (0.35 mg, 1.27 mmol) as prepared according to the method described in example 22, and 1,1′-carbonyl-diimidazole (0.31 g, 1.91 mmol) in DMF (8 ml) was stirred at room temperature for 3 h and subsequently N-hydroxy-cyclopropanecarboxamidine (0.19 g, 1.91 mmol) was added. The reaction mixture was stirred at 80° C. for 20 h and evaporated. Acetic acid (10 ml) was added and the stirred mixture was heated under reflux conditions for 2 h. Aqueous work-up, column chromatography on silica gel (ethyl acetate/hexane 3:2) and crystallization from ethyl acetate/hexane yielded the title compound (36 mg, 9%) as an off-white solid, m.p. 94° C. and MS: m/e=340.3 (M+H+).

1. stirringThe reaction mixture was stirred at 80° C. for 20 h
2. customevaporated
3. additionAcetic acid (10 ml) was added
4. temperaturethe stirred mixture was heated under reflux conditions for 2 h
5. customAqueous work-up, column chromatography on silica gel (ethyl acetate/hexane 3:2) and crystallization from ethyl acetate/hexane