関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(2,3-Epoxypropyl)-2-nitroimidazole | HCID 334973 | — |
| 反応物 | 3-Bromopropylazanium;bromide | HCID 11031334 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-(2-Nitro-1-imidazolyl)-3-(3-bromopropylamino)-2-propanol hydrobromide | HCID 14621567 | 119.6% |
反応手順
A solution containing 3-bromopropylammonium bromide (6.47 g, 29.6 mmol) and sodium hydroxide (1.18 g, 29.5 mmol) in ethanol (40 cm3) was stirred at 20° C.; after 1 hour, diethyl ether (40 cm3) was added and the mixture filtered. 1-(2,3-epoxypropyl)-2-nitroimidazole (5.00 g, 29.6 mmol) was added to the filtrate and the solution heated to reflux for 45 minutes. The reaction mixture was then treated with decolourising charcoal (0.5 g), filtered, concentrated under reduced pressure and treated with aqueous hydrobromic acid (48% w/w HBr, 2.0 cm3). The solid which appeared upon refrigeration was recrystallised from aqueous ethanol to give 1-(2-nitro-1-imidazolyl)-3-(3-bromopropylamino)-2-propanol hydrobromide (6.87 g, 59.9%) as a hygroscopic yellow crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05098921 |
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| 出典データセット | uspto-grants-1992_03 |
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| ORD ID | ord-afdc90622a674874b9d06aa2d0a323fd |
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| 出典メモ | uspto-grants-1992_03 |
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