関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5,5-Diphenylhydantoin | HCID 1775 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1-(2-Chloroethyl)-2-methyl-5-nitroimidazole | HCID 83210 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-[2-(2-Methyl-5-nitro-1-imidazolyl)ethyl]-5,5-diphenylhydantoin | HCID 21491662 | — |
反応手順
1.4 Parts of 1-(2-chloroethyl)-2-methyl-5-nitroimidazole is mixed with 2.5 parts of the sodium salt of 5,5-diphenylhydantoin and 75 parts of dimethylformamide is added under nitrogen. The mixture is heated on a steam bath for 1 hour and then 10 parts of methanol is added and heating is continued for an additional 4 hours. The solvent is then evaporated on the steam bath under a stream of nitrogen to leave a residual mixture of solid and oil. The residue is mixed with toluene and filtered to remove some insoluble material. The toluene solution is diluted to a volume of 250 parts and washed with a mixture of 25 parts of sodium bicarbonate and 120 parts of water. The toluene solution is then washed with water and dried over magnesium sulfate and the solvent is evaporated to leave a solid residue. This is digested in warm ether and then cooled and the solid is separated by filtration. The solid is recrystallized from ethanol to give 3-[2-(2-methyl-5 -nitro-1-imidazolyl)ethyl]-5,5-diphenylhydantoin melting at about 209°-210.5° C. This compound has the following formula ##STR8##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03997572 |
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| 出典データセット | uspto-grants-1976_12 |
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| ORD ID | ord-0a374b24630d4ac4b5faf421d94ab167 |
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| 出典メモ | uspto-grants-1976_12 |
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