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N-Iodosuccinimide → 5-Iodo-6-methoxynaphthalene-2-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | 6-Methoxynaphthalene-2-carbonitrile | HCID 349173 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 5-Iodo-6-methoxynaphthalene-2-carbonitrile | HCID 117902664 | — |
反応手順
A mixture of 6-methoxynaphthalene-2-carbonitrile (1.0 g, 5.5 mmol), N-iodosuccinimide (1.4 g, 6.0 mmol) in ACN (10 ml) and TFA (125 μl) is stirred at RT for 4 h. A saturated aqueous solution of sodium hydrogencarbonate is added and the mixture extracted with DCM. The combined organic layers are extracted with an aqueous solution of sodium thiosulfate, dried over MgSO4 and concentrated in vacuo. The product is purified by RP HPLC. Yield: 1.68 g (99%). HPLC-MS: tR=1.32 min (METHOD—1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09249151B2 |
| 出典データセット | uspto-grants-2016_02 |
| ORD ID | ord-2d2b54f742be4a319fc19536e0ca3c0d |
| 出典メモ | uspto-grants-2016_02 |