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Hydrochloric Acid → HCID 54423814、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,1-Dichloroethane | HCID 6365 | — |
| 反応物 | 4-Fluoro-2-(trifluoromethyl)aniline | HCID 67853 | — |
| 反応物 | Methyl 3-(chlorosulfonyl)propanoate | HCID 4962888 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 54423814 | HCID 54423814 | — |
反応手順
8.96 g (50 mmol) of 4-fluoro-2-trifluoromethylaniline is dissolved in 100 ml of pyridine and under cold conditions combined under stirring with 9.52 g (50 mmol) of 3-chlorosulfonylpropionic acid methyl ester (98.5%). The mixture is agitated for 20 minutes, heated for 4 hours to 40° C., and the pyridine is exhausted under vacuum. The residue is distributed between dichloroethane and 4N hydrochloric acid. The organic solution is washed with water, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is purified by column chromatrography on silica gel. The title compound is eluted with ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05210290 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-d18b19c5760f4c7a9fe769c7ee4fafca |
| 出典メモ | uspto-grants-1993_05 |