反应详情

To a solution of 1-[3-(2-guanidinothiazol-4-yl)-cyclohexylamino]-2-methoxycyclobutene-3,4-dione (0.35 g.) in 60 ml. of methanol/chloroform (50:50 v/v) was added 1,4-diaminobutane (0.044 g.) in methanol (1 ml.). The solution was heated under reflux for 16 hours during which time a precipitate formed. The reaction mixture was cooled and the solid precipitate collected and washed with methanol (1 ml.) and ether (2 ml.) to give, as an off-white powder, 1,4-bis{1-[3-(2-guanidinothiazol-4-yl)cyclohexylamino]-3,4-dioxocyclobutenylamino}butane. The carbon-13 magnetic resonance spectrum (δ relative to tetramethylsilane) in d6 -DMSO included one carbon singlets at 182.3, 174.8, 167.7, 167.0, 156.7, 155.3, 100.3 and 52.4 together with a series of singlets from 42.9 to 24.0 p.p.m. (the latter group of signals includes the resonances due to the solvent).

1. temperatureThe solution was heated
2. temperatureunder reflux for 16 hours during which time a precipitate
3. customformed
4. temperatureThe reaction mixture was cooled
5. customthe solid precipitate collected
6. washwashed with methanol (1 ml.) and ether (2 ml.)