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2-Methylbenzenesulfonic acid → 3-Amino-1-(3-chloro-4-bromobenzyl)-pyrazol-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| 反応物 | beta-Aminobeta-ethoxyacrylic acid ethyl ester | HCID 278451 | — |
| 反応物 | [(4-Bromo-3-chlorophenyl)methyl]hydrazine | HCID 20495799 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Amino-1-(3-chloro-4-bromobenzyl)-pyrazol-5-one | HCID 20367220 | — |
反応手順
48.8 g of 4-bromo-3-chlorobenzylhydrazine are added dropwise under nitrogen to a solution of 33.2 g of β-amino-β-ethoxyacrylic acid ethyl ester and 1.5 g of toluenesulphonic acid in 150 ml of ethanol. After stirring for a further two hours, the mixture was left to stand and the compound identified above began to crystallise out after four hours. It was filtered off and twice recrystallised from ethanol. Melting point: 145°-146°, 23 g (37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04061653 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-b1355b9f8c884251b2a602436be410aa |
| 出典メモ | uspto-grants-1977_12 |