関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | tert-Butylhydrazine monohydrochloride | HCID 81889 | — |
| 反応物 | 1-Cyclohexenecarbonyl chloride | HCID 142066 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine | HCID 15451994 | — |
反応手順
To a stirred suspension of t-butylhydrazine hydrochloride (0.86 g, 0.007M) in toluene (30 ml) was added 50% sodium hydroxide (0.55 g, 0.007M). After 15 minutes, the mixture was cooled to 5° C. and cyclohexenylcarbonyl chloride (1.0 g, 0.007M) and 50% sodium hydroxide (0.55 g, 0.007M) were added separately and simultaneously so as to maintain the reaction temperature below 10° C. After the addition, the reaction mixture was allowed to warm to room temperature and stirred for 1 hour. The mixture was diluted with hexane and the solid product isolated by filtration. This product (1.2 g, 0.006M) was dissolved in toluene (30 ml) and cooled on ice while stirring. To this mixture was added benzoylchloride (1.0 g, 0.007M) and 50% sodium hydroxide (1.3 g, 0.007M) simultaneously. After addition, the mixture was stirred for 1/2 hour, diluted with hexane and the solid product, N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine, was isolated by filtration.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424333 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-afd9ef446bce4af0b9c4f598804702b2 |
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| 出典メモ | uspto-grants-1995_06 |
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