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O,O-Dipyridin-2-yl carbonothioate → 2-Ethoxy-8-isothiocyanato-1,4-dihydronaphthalene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O,O-Dipyridin-2-yl carbonothioate | HCID 719784 | — |
| 反応物 | 7-Ethoxy-5,8-dihydronaphthalen-1-amine | HCID 23066996 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Ethoxy-8-isothiocyanato-1,4-dihydronaphthalene | HCID 86609612 | — |
反応手順
A solution of the product of Example 1E (200 mg, 1.06 mmol) in dichloromethane (2.5 mL) was added to a solution of O,O-dipyridin-2-yl thiocarbonate (246 mg, 1.06 mmol) in dichloromethane (5 mL) at room temperature. After stirring at room temperature for 18 hours, the mixture was concentrated, then filtered through silica gel and eluted with 5% ethyl acetate-hexane. Evaporation of the filtrate in vacuo afforded the title compound as a pale pink solid, 225 mg (92%). 1H NMR (DMSO-d6) δ 7.21-7.27 (m, 3H), 4.86 (t, 1H, J=3.6 Hz), 3.81 (q, 2H, J=7.0 Hz), 3.49 (q, 2H, 4.4 Hz), 3.35 (t, 2H, J=5.2 Hz), 1.27 (t, 3H, J=7.0 Hz); MS (DCI+) m/z 232 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902236B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-3c6d5ac5b5b249a09758f315337759dd |
| 出典メモ | uspto-grants-2011_03 |