関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Salicylate | HCID 4133 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Methanol--water (1/1) | HCID 22242641 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Hydroxybenzoic acid 2-(2-hydroxybenzoyl)hydrazide | HCID 65303 | — |
反応手順
0.5 kg (10 mol) hydrazine hydrate was heated with 3.040 kg (20 mol) salicylic acid methyl ester and 2.714 kg vaseline in a protective gas such as nitrogen or argon in the apparatus according to the invention. The water-methanol mixture produced was continuously distilled-off from the reaction mixture. After about three hours, the reaction temperature had risen to 120° C. and approximately half of the quantity of methanol expected theoretically and the entire amount of water were distilled off (0.5 kg). The hydrazide was present in the vaseline as a crystal product in paste. The heating was continued after 30 g boron trioxide was added and the temperature was kept at 150° C. The remaining methanol (0.320 kg) was distilled off. After about three hours, the reaction was complete as determined by the amount of methanol distilled off.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04550204 |
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| 出典データセット | uspto-grants-1985_10 |
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| ORD ID | ord-fa763f0050c54319865f6bc7d5d33c9a |
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| 出典メモ | uspto-grants-1985_10 |
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