関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylphenylhydrazine monohydrochloride | HCID 12504 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | Propanoyl chloride, 3-bromo- | HCID 84944 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-Methylphenyl)pyrazolidin-3-one | HCID 1913485 | 19,455.801% |
反応手順
10 g of p-tolylhydrazine hydrochloride are dissolved in 100 ml of anhydrous CH2Cl2. The solution is cooled to 0° C. and 19 ml of DBU and then 6.5 mg of 3-bromopropionyl chloride are added. The mixture is stirred at ambient temperature for one hour. The reaction medium is poured onto water, extraction is carried out with CH2Cl2 and then purification is carried out by chromatography on a silica column eluted with an AcOEt/petroleum ether (v/v; 50/50) mixture. 1.3 g of crystals are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07390818B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-e0d1fe6a07a74c78a3121edd965e5815 |
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| 出典メモ | uspto-grants-2008_06 |
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