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1-(4-Chloro-2-phenyl-thieno[3,2-c]pyridin-7-yl)-ethanol → 1-(4-Chloro-2-phenyl-thieno[3,2-c]pyridin-7-yl)-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(4-Chloro-2-phenyl-thieno[3,2-c]pyridin-7-yl)-ethanol | HCID 18446511 | — |
| 触媒 | HCID 178419074 | HCID 178419074 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-Chloro-2-phenyl-thieno[3,2-c]pyridin-7-yl)-ethanone | HCID 18446512 | — |
反応手順
To a suspension of 1-(4-chloro-2-phenyl-thieno[3,2-c]pyridin-7-yl)-ethanol 96 (92 mg, 0.32 mmol) and 168 mg of powdered 4A molecular sieves in dichloromethane (35 mL) was added TPAP (11 mg, 0.03 mmol). The resultant mixture was stirred at room temperature for 1 h. After this time, the reaction mixture was diluted with dichloromethane and washed with saturated aqueous sodium thiosulfate (1×) and saturated aqueous copper sulfate (1×). The organic layer was dried over Na2SO4, filtered, and the filtrate was purified by silica gel column chromatography (eluent: hexane:EtOAc, 17:3) to give 97. 1H NMR (400 MHz, CDCl3) δ: 2.79 (s, 3H), 7.40-7.53 (m, 3H), 7.75 (s, 1H), 7.78-7.83 (m, 2H), 8.83 (s, 1H). MS (EI) m/z (M+H+) 288.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07635695B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-b0eafc1a48e74bdeb0e02867d7465f17 |
| 出典メモ | uspto-grants-2009_12 |