関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 5-Nitroindoline | HCID 36219 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Methylsulfonyl)-5-nitroindoline | HCID 2918213 | 92.5% |
反応手順
To a solution of 300 mg (1.83 mmol) of 5-nitroindoline in 20 mL of dichloromethane were added 141 μL (2.74 mmol) of methanesulfonyl chloride and 382 μL (2.74 mmol) of triethylamine, and the mixture was stirred for 2 hours at room temperature. 141 μL (2.74 mmol) of methanesulfonyl chloride and 255 μL (1.83 mmol) of triethylamine were further added to the reaction mixture, and the mixture was stirred for 2 hours at room temperature. Then, water was added to the reaction mixture and the mixture was extracted with dichloromethane. The organic layer was washed with saturated saline solution and dried over with anhydrous sodium sulfate. The solvent was removed under reduced pressure and the residue was treated with diethyl ether, then, the precipitates were collected by filtration to give 410 mg (92%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07932250B2 |
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| 出典データセット | uspto-grants-2011_04 |
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| ORD ID | ord-81b4031322874844b4840040276ae71d |
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| 出典メモ | uspto-grants-2011_04 |
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