関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | [2-(6-chloro-8-nitro-9H-beta-carbolin-7-ylsulfanyl)-ethyl]-dimethyl-amine | HCID 67166181 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-chloro-7-(2-dimethylamino-ethylsulfanyl)-9H-beta-carbolin-8-ylamine | HCID 67164517 | 107% |
反応手順
A 50 ml round-bottom flask with a magnetic stirrer was charged with [2-(6-chloro-8-nitro-9H-β-carbolin-7-ylsulfanyl)-ethyl]-dimethyl-amine (106 mg, 0.30 mmol) in 8 ml of anhydrous ethanol. To the resulting orange mixture at RT was added 0.33 M aqueous ammonium chloride (1.95 ml, 0.64 mmol) and iron powder (540 mg, 9.67 mmol). The reaction mixture was heated to 60° C. and stirred vigorously for 20 hr. Next, the mixture was cooled to RT, diluted with ethyl acetate (20 ml) and activated charcoal (ca. 150 mg) was added. The resulting mixture was filtered through a pad of celite and the resulting filtrate concentrated to afford 103 mg of 6-chloro-7-(2-dimethylamino-ethylsulfanyl)-9H-β-carbolin-8-ylamine as a yellow solid. The crude product was used directly in the coupling step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727985B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-6cee690533f34e0b838930aeaf183eee |
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| 出典メモ | uspto-grants-2010_06 |
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