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Chloroform → 5-Formyl-2-thiophenecarboxylic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 5-Methylthiophene-2-carboxylic acid | HCID 74713 | — |
| 触媒 | Tungsten | HCID 23964 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 5-Formyl-2-thiophenecarboxylic Acid | HCID 818882 | — |
反応手順
2-Methyl thiophen-5-carboxylic acid was dissolved in carbon tetrachloride (150 ml.) and chloroform (10 ml.) and AZDN (0.5g.) was added. The mixture was refluxed over a 150 watt tungsten spotlight. Two molar equivalents of bromine as a 30% v/v solution in carbon tetrachloride were slowly added. A precipitate was formed but the mixture continued to take up bromine. After the addition of the two molar equivalents, solvent was boiled off until the volume was 100 ml. and the product treated with sodium carbonate solution with gentle heating for two hours to obtain 2-formyl thiophen-5-carboxylic acid in the form of a yellow solid after acidification, extraction and removal of the solvent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03947336 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-b6867c0130184750802e3e579b65ce10 |
| 出典メモ | uspto-grants-1976_03 |