関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | m-Bromobenzohydrazide | HCID 520941 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | Benzoic acid, m-bromo-, benzoylhydrazide | HCID 52256 | 96% |
反応手順
Next, 5.0 grams (23 mmol) of the 3-bromobenzoylhydrazine obtained in (i) were placed into a 300 mL, three-neck flask, 10 mL of N-methyl-2-pyrrolidone was added thereto, and the mixture was stirred. A mixed solution of 10 mL of N-methyl-2-pyrrolidone and 3.2 mL (28 mmol) of benzoyl chloride were dripped into this mixture through a 50 mL dropping funnel. After completion of the dripping, the mixture was heated and stirred at 80° C. for 3 hours, and the contents of the flask were reacted together. After the reaction was completed, a solid was precipitated out with the addition of water to the reaction solution. A solid was obtained by suction filtration of the precipitate solid. The obtained solid was washed with approximately 1 L of water and removed by suction filtration. After the suction-filtered solid was washed with methanol and a solid was removed by suction filtration, 7.1 grams of a white-colored solid, which was the objective of the synthesis process, were obtained at a yield of 96%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08221904B2 |
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| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-3792f1be691042f3aac9c9884be17c84 |
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| 出典メモ | uspto-grants-2012_07 |
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