関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 5-Bromo-8-nitroisoquinoline | HCID 816983 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Bromoisoquinolin-8-amine | HCID 16218302 | 68.1% |
反応手順
A 3-neck flask was charged with 5-bromo-8-nitroisoquinoline (4 g, 15.8 mmol) and dissolved in MeOH (50 mL). A condenser was affixed and the mixture was heated to 100° C. Aqueous (20 mL) solution of ammonium chloride (4.12 g, 79 mmol) was added slowly, followed by iron powder (3 g, 53.7 mmol). The heterogeneous mixture was stirred at 100° C. for 3 h. LCMS confirmed complete reduction to the amine. The mixture was filtered and the solution was concentrated under reduced pressure to give a brown solid as crude product (2.4 g, 68%). LCMS showed an m/z of 225.0/223.0 with a retention time of 0.767 min, method [1].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08450363B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-15a26c3bc9b747d68e72992d617d4d24 |
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| 出典メモ | uspto-grants-2013_05 |
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