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Ammonium Chloride → 5-Chlorothiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2,5-Dichlorothiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide | HCID 86600992 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Chlorothiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide | HCID 86071418 | 90.9% |
反応手順
To a solution of 2,5-dichlorothiophene-3-sulfonic acid [2-(4-fluorophenyl)ethyl]-methyl-amide (1.14 g) in tetrahydrofuran (10 mL) was added dropwise a solution of 1.59M n-butyl lithium-hexane (2.3 mL) on an ice bath. After stirring for 30 minutes, an aqueous solution of saturated ammonium chloride was poured. After diluting with water, the solution was extracted with ethyl acetate. After the organic layer was washed with saturated sodium chloride water, and was dried with anhydrous sodium sulfate. The residue that was obtained upon removing the solvent by evaporation was purified by silica gel column chromatography (hexane/ethyl acetate), and the title compound (pale yellow oily substance) (939 mg) was obtained (contains impurities).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07217723B2 |
| 出典データセット | uspto-grants-2007_05 |
| ORD ID | ord-3c32f313937a495e8ccdb488b1af34ac |
| 出典メモ | uspto-grants-2007_05 |