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Methanesulfonyl chloride → 2-Iodo-4-nitrobenzyl Methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | (2-Iodo-4-nitrophenyl)methanol | HCID 279258 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Iodo-4-nitrobenzyl Methanesulfonate | HCID 57961681 | 80.1% |
反応手順
To a solution of (2-iodo-4-nitrophenyl)methanol (6.01 g, 21.5 mmol) in methylene chloride (50 mL) was added N,N-diisopropylethylamine (7.50 mL, 43.1 mmol) and methanesulfonyl chloride (1.83 mL, 23.7 mmol) at 0° C. The reaction solution was stirred at same temperature for 2 hours. The reaction was quenched with water, and aqueous layer was extracted with DCM once. The combined organic solutions were washed with brine, dried over Na2SO4, filtered and concentrated The crude product was purified by flash column chromatography to give the desired product (6.15 g, 80%). LCMS calculated for C8H91NO5S (M+H)+: m/z=358.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871753B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-f70d53f84da043fe9c4d78d92e66e455 |
| 出典メモ | uspto-grants-2014_10 |