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2-Dimethylaminopyridine → 2,3-Dihydro-1h-inden-2-yl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2-Indanol | HCID 77936 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,3-Dihydro-1h-inden-2-yl methanesulfonate | HCID 255221 | 78% |
反応手順
2-Indanol (20.00 g, 149.5 mmol) and diisopropylethylamine (21.2 g, 164 mmol) was stirred in dichloromethane (300 mL) at 0° C. Methanesulfonyl chloride (18.78 g, 164 mmol) and dimethylaminopyridine (1.80 g) were added simultaneously and stirring continued at room temperature for 18 h. Solution was evaporated, partitioned between ethyl acetate and water, and the organic phase separated. This was washed with NaHCO3 (sat) and with citric acid solution (5%) and dried over MgSO4. The filtered solution was concentrated and the resultant solid recrystallized from isopropanol-EtOH (3:1) to give off-white crystals (24.6 g, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486984B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-8a773c1aeae7433abb88a6f5b83d4413 |
| 出典メモ | uspto-grants-2013_07 |