関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | 2-Thiopheneacetyl chloride | HCID 162362 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 7-amino-3-(1-methyl-1H-tetrazol-5-yl)vinyl-3-cephem-4-carboxylic acid | HCID 131711472 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7-(2-thienylacetamido)-3-(1-methyl-1H-tetrazol-5-yl)vinyl-3-cephem-4-carboxylic acid | HCID 131711471 | 101.1% |
反応手順
In 40 ml of water were dissolved 416 mg of 7-amino-3-(1-methyl-1H-tetrazol-5-yl)vinyl-3-cephem-4-carboxylic acid and 660 mg of sodium hydrogencarbonate. To the solution was added 10 ml of acetone and further added dropwise with stirring at 0°-5° C., 20 ml of an acetone solution containing 323 mg of 2-thienylacetyl chloride. The mixture was stirred for 30 minutes under ice-cooling and for additional 3 hours at room temperature. The acetone was distilled off at room temperature under reduced pressure. The residual solution was washed with ether, adjusted to pH 2.0 with 10% hydrochloric acid and extracted with ethyl acetate. The extract was washed with an aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The ethyl acetate was removed under reduced pressure, and, upon washing the residue with ether, there was obtained 590 mg of 7-(2-thienylacetamido)-3-(1-methyl-1H-tetrazol-5-yl)vinyl-3-cephem-4-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04147863 |
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| 出典データセット | uspto-grants-1979_04 |
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| ORD ID | ord-29b0d6884b9a4451b5e5cdca3673477c |
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| 出典メモ | uspto-grants-1979_04 |
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