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 | 2,4-Difluorobenzoic acid hydrazide | HCID 2736922 | — |
| 反応物 | 2-(Phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride | HCID 70089441 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2,4-Difluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide | HCID 70088569 | 42% |
反応手順
A suspension of 15.3 g (0.058 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 125 ml chloroform was treated with 58.1 ml 1N aqueous sodium hydoxide. 18 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. The resulting colorless oil was stirred together with 10.0 g (0.058 mol) 2,4-difluorobenzoic acid hydrazide in 110 ml chloroform over night at 50° C. The resulting precipitate was filtered off and dried. A yield of 8.50 g (42%) 2,4-difluoro-benzoic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white solid. MS m/e (%): 354 (M+H+, 100).
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-2ea8e458666b4f0e9dd79ae524c2a16a |
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| 出典メモ | uspto-grants-2002_03 |
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