関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-Methyl-1,2,3-thiadiazole-5-carboxylic acid | HCID 1381992 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | (4-Methyl-1,2,3-thiadiazol-5-yl)(phenyl)methanone | HCID 12298991 | 97% |
反応手順
To 2.0 g (15 mimol) of thionyl chloride was added 0.50 g (3.5 mmol) of 4-methyl-1,2,3-thiadiazole-5-carboxylic acid. After heating the mixture with stirring for 2 hours, the thionyl chloride was distilled off under reduced pressure, and the residue was added to a solution of 1.8 g (15 mmol) of aluminum chloride in 20 ml benzene and made to react with heating for 3 hours. After the reaction was completed, the reaction mixture was poured into ice water, the objective product was extracted with ethyl acetate, the organic layer was ashed with a saturated aqueous solution of sodium chloride and dried, the solvent was distilled off under educed pressure, and the residue was purified by silica gel column chromatography using 4:1 mixture of n-hexane and ethyl acetate. Thus, 0.69 g of the objective compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06194444B1 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-2b7872b2bf45499d919201ef99717658 |
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| 出典メモ | uspto-grants-2001_02 |
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