関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Putrescine | HCID 1045 | — |
| 反応物 | Chloroform methanol | HCID 21584188 | — |
| 反応物 | HCID 178493670 | HCID 178493670 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178512615 | HCID 178512615 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04342765 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-0263457af80e450a9fa8b828f0f63347 |
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| 出典メモ | uspto-grants-1982_08 |
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