関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | 2-Mepp | HCID 91965 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 2-Chloro-1-(4-o-tolylpiperazin-1-yl)ethanone | HCID 4741212 | 83% |
反応手順
Chloroacetyl chloride (4.5 ml, 56.6 mmol) is added dropwise to a solution of 1-o-tolylpiperazine (8.31 [lacuna], 47.2 mmol) and calcium carbonate (14.2 g, 142 mmol) in methyl ethyl ketone (100 ml) cooled to 0° C. The reaction mixture is stirred at this temperature for 1 h 30 and is then filtered through Celite. The Celite is rinsed several times with ethyl acetate and 3M sodium hydroxide solution. The two phases of the filtrate are then separated and the organic phase is dried over magnesium sulfate, filtered and concentrated to give the expected product in the form of a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05789412 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-6f100b1ebd584b75824b3201336f9e84 |
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| 出典メモ | uspto-grants-1998_08 |
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