関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | (4-Methylphenyl)hydrazine | HCID 10875 | — |
| 反応物 | Methyl 4-ethoxy-2-oxobut-3-enoat | HCID 54443622 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 1-(4-methylphenyl)-pyrazole-5-carboxylate | HCID 14129278 | — |
| 生成物 | Methyl 1-(4-methylphenyl)-1H-pyrazole-3-carboxylate | HCID 14129279 | — |
反応手順
12.5 g of p-tolylhydrazine in 150 ml of glacial acetic acid were added to a solution of 16 g of methyl 4-ethoxy-2-oxobut-3-enoat in 100 ml of glacial acetic acid at 50° C. The mixture was stirred at 100° C. for 5 hours, poured into 1 liter of water, and extracted twice with 100 ml of ethyl acetate. The organic phase was washed with saturated NaHCO3 solution and subsequently with water, and dried. After evaporating in a water-pump vaccum, the mixture was separated by distillation in a high vacuum. 4.1 g of methyl 1-(4-methylphenyl)-pyrazole-5-carboxylate of boiling point 116°-120° C./0.01 torr (example 8) and 5.3 g of methyl 1-(4-methylphenyl)-pyrazole-3-carboxylate of boiling point 138°-142° C./0.01 torr were obtained. The compounds were characterized by 1H NMR spectroscopy.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04891057 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-e8f7fbe2e1b24b86bf2ee8929eb6660b |
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| 出典メモ | uspto-grants-1990_01 |
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