関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | HCID 178527775 | HCID 178527775 | — |
| 生成物 | 3-Methyl[1,3]thiazolo[3,2-a]benzimidazole | HCID 828285 | — |
反応手順
2-Mercaptobenzoimidazole (15.0 g) was added to EtOH (100 ml) solution of KOH (6.60 g), and the mixture was heated under reflux for 1 hour. After cooling to room temperature, this was mixed with 2-chloroacetone (7.96 ml) and stirred overnight. The reaction solution was mixed with EtOAc and stirred, the insoluble matter was removed by filtration and then the solvent was evaporated under a reduced pressure. The thus obtained oily material was dissolved in concentrated sulfuric acid (100 ml) and stirred at room temperature for 6 hours. The reaction solution was poured into ice water and then neutralized with 28% NH3 aqueous solution, and the resulting precipitate was collected by filtration. This was recrystallized from MeOH to obtain the title compound (9.60 g) as light brown crystals. (J. O. C., 29 (4), 865-9 (1964))
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06642264B1 |
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| 出典データセット | uspto-grants-2003_11 |
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| ORD ID | ord-e71f72a8e04b47a687b2f30222c34596 |
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| 出典メモ | uspto-grants-2003_11 |
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