関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitrobenzoyl chloride | HCID 11875 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N'-t-butyl-N-(2-pyridinecarbonyl)hydrazine | HCID 15767542 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N'-t-butyl-N-(2-pyridinecarbonyl)-N'-(2-nitrobenzoyl)hydrazine | HCID 15767544 | 22.6% |
反応手順
A solution of N'-t-butyl-N-(2-pyridinecarbonyl)-hydrazine (1.0 g, 0.00518 mol) in 20 ml of toluene was treated dropwise simultaneously with a solution of sodium hydroxide (1.24 g of 50% aqueous solution) in 5 ml of water and 2-nitrobenzoyl chloride (0.96 g). The resulting mixture was stirred at 23° C. overnight. Water was added and the mixture was extracted with ether. A second extraction was performed with methylene chloride and the combined organic extracts were dried over magnesium sulfate. Evaporation afforded 0.4 g of N'-t-butyl-N-(2-pyridinecarbonyl)-N'-(2-nitrobenzoyl)hydrazine as a yellow solid: m.p. 137°-140° C.
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-70c0923c5e2848879bce03b94ac269c2 |
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| 出典メモ | uspto-grants-1995_06 |
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