関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5-Methyl-2-furohydrazide | HCID 4159250 | — |
| 反応物 | 2-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride | HCID 70089441 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-Methyl-furan-2-carboxylic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide | HCID 86757844 | 82.8% |
反応手順
A suspension of 85.0 g (0.32 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 700 ml chloroform was treated with 320 ml 1N aqueous sodium hydroxide. 100 ml of a saturated aqueous sodiumbicarbonate solution was added and the mixture was extracted with chloroform. The extracts were combined and dried with sodium sulfate and the solvents were distilled off under reduced pressure. 17.8 g (0.078 Mol) of the resulting colorless oil was stirred together with 9.15 g (0.065 mol) 5-methyl-furan-2-carboxylic acid hydrazide in 115 ml chloroform for 24 hours at 50° C. The resulting precipitate was filtered off and dried. 17.3 g of 5-methyl-furan-2-carboxylic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white crystals. Mp.: 219-220° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06355653B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-7ecc062fc0854a2c86eb72796e15cb16 |
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| 出典メモ | uspto-grants-2002_03 |
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