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Acetonitrile → 3-Phenylureido-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Phenyl isocyanate | HCID 7672 | — |
| 反応物 | 4-Hydrazinobenzenesulfonic acid | HCID 66825 | — |
| 反応物 | Ethylbeta-amino-beta-ethoxy acrylate | HCID 86736826 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 3-Phenylureido-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt | HCID 86736830 | — |
反応手順
Into 30 ml of acetonitrile was dissolved 4 g of ethylβ-amino-β-ethoxy acrylate, and 3 g of phenyl isocyanate was added thereto. The resulting solution was allowed to stand at room temperature for 24 hours. Into a mixed solution of 20 ml of methanol, 6 g of triethylamine and 5 ml of glacial acetic acid there was dissolved 4.7 g of p-sulfophenyl hydrazine, and the above solution, in which the esterification reaction had been completed, was added thereto. The resulting solution was allowed to stand at room temperature for 5 days. The crystals obtained were collected, washed with acetonitrile, and then recrystallized from methanol; thus 7.5 g of crystals of a melting point of 240° to 242° C. was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04188489 |
| 出典データセット | uspto-grants-1980_02 |
| ORD ID | ord-8e38e84ac0384cd49f4bbe68de885163 |
| 出典メモ | uspto-grants-1980_02 |