関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Fluoro-2-(trifluoromethyl)aniline | HCID 67853 | — |
| 反応物 | Methyl (chlorosulfonyl)acetate | HCID 11435213 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl ester | HCID 15057604 | — |
反応手順
5 g (27.64 mmol) of 4-fluoro-2-(trifluoromethyl)-aniline is dissolved in 25 ml of dry pyridine and the solution is cooled to 0° C. A solution of 4.82 g (27.4 mmol) of chlorosulfonyl acetic acid methyl ester in 20 ml of dichloromethane is instilled in the cooled solution in the course of about 10 minutes with the temperature being maintained. Then it is stirred for 6 hours at room temperature. The reaction solution is then diluted with 100 ml of dichloromethane, the pyridine is shaken out with 2N hydrochloric acid, the organic phase is dried on magnesium sulfate, filtered and evaporated to dryness. The residue is crystallized from diethyl ether/hexane yield is obtained as a crystallizate. Melting point 84°-86° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05130119 |
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| 出典データセット | uspto-grants-1992_07 |
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| ORD ID | ord-a33c0f384d364543b7c03887fdc98fb1 |
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| 出典メモ | uspto-grants-1992_07 |
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