반응 #94858

반응 방정식

1-[3-(2-guanidinothiazol-4-yl)cyclohexylamino]-2-methoxycyclobutene-3,4-dione

methanol chloroform

2-guanidino-4-(3-aminocyclohexyl)thiazole

→

1,2-bis[3-(2-guanidinothiazol-4-yl)cyclohexylamino]cyclobutene-3,4-dione

용매

methanol

반응 조건

후처리

1. 1
   온도After heating
2. 2
   온도under reflux for 6 hours
3. 3
   농축the reaction mixture was concentrated
4. 4
   온도cooled

실험 절차

To a solution of 1-[3-(2-guanidinothiazol-4-yl)cyclohexylamino]-2-methoxycyclobutene-3,4-dione (0.1 g.) in 15 ml. of methanol/chloroform (50:50 v/v) was added a solution of 2-guanidino-4-(3-aminocyclohexyl)thiazole (0.07 g.) in methanol (3 ml.) and the resulting solution was allowed to stand at room temperature for 6 hours. After heating under reflux for 6 hours, the reaction mixture was concentrated and cooled to give, as a white amorphous solid, 1,2-bis[3-(2-guanidinothiazol-4-yl)cyclohexylamino]cyclobutene-3,4-dione. The carbon-13 magnetic resonance spectrum (δ relative to tetramethylsilane) in d6DMSO included one carbon singlets at 181.9, 175.0 167.0, 156.8, 155.4, 100.3, 52.4 and a series of signals from 52.4 to 24.1 (including resonances attributable to solvent) p.p.m.

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