関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | N-[4-cyano-3-(trifluoromethyl)phenyl]-2,3-dihydroxy-2-methylpropanamide | HCID 9882395 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[4-cyano-3-trifluoromethyl-phenyl]-2-hydroxy-3-methanesulfonyloxy-2-methyl-propionamide | HCID 12148451 | — |
反応手順
A solution of 46 g (0.16 mol) of N-[4-cyano-3-trifluoromethyl-phenyl]-2,3-dihydroxy-2-methyl-propionamide in 1 1 of dichloromethane and 46 ml (0.57 mol) of dry pyridine was cooled to 0° C. and 46 ml (0.59 mol) of methanesulfonyl chloride was added dropwise. The mixture was stirred at 0° C. for 5 h, then washed three times with 500 ml of saturated aqueous sodium hydrogen carbonate, 500 ml of 10% aqueous hydrochloric acid and 500 ml of brine. The organic layer was dried over sodium sulfate and concentrated in vacuum. The residue was crystallized with 200 ml of petroleum ether, which has a boiling range of 40–70° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07199257B1 |
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| 出典データセット | uspto-grants-2007_04 |
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| ORD ID | ord-b35866d175fd4d758effefbba81c681b |
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| 出典メモ | uspto-grants-2007_04 |
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