関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chloral alcoholate | HCID 10587 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 3-Bromo-o-toluidine | HCID 123538 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Bromo-7-methyl-1H-indole-2,3-dione | HCID 11230188 | 61.2% |
反応手順
Chloral alcoholate (0.43 g, 1.05 eq) and Na2SO4(2.84 g, 20 mmol) were dissolved in 10 mL water. 3-Bromo-2-methylaniline (0.33 g, 1.77 mmol) was added to the solution followed by 0.16 mL conc. HCl aqueous solution and NH2OH.HCl (0.38 g, 3.0 eq). The mixture was refluxed for 15 min and stirring was continued for additional 1 hr at RT. The precipitate was collected by filtration, washed with water and dried under vacuum. This precipitate was dissolved in 1 mL H2SO4 and the solution was heated (80° C.) for 15 min. After cooling down to RT, the mixture was poured into ice-water mixture and the precipitate was collected, washed with water and dried under vacuum to give the title compound (0.26 g, 61%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871718B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-3f4e562708fc4e11891c163b21f062ff |
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| 出典メモ | uspto-grants-2014_10 |
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