関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 反応物 | 2-Nitromethylene-thiazolidine | HCID 3835583 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Chloro-5-[[2-(nitromethylene)-3-thiazolidinyl]methyl]pyridine | HCID 54565385 | 29.8% |
反応手順
2-Nitromethylenethiazolidine (2.9 g) was dissolved in dry acetonitrile (30 ml), and 60% sodium hydride (0.9 g) was added at room temperature in a stream of nitrogen. Subsequently, the mixture was stirred at room temperature until the generation of hydrogen ceased. Then, a solution of 2-chloro-5-pyridylmethyl chloride (3.2 g) in dry acetonitrile (5 ml) was added at room temperature, and the mixture was stirred at room temperature for 1 day. Acetonitrile was then distilled off under reduced pressure, and dichloromethane was added to the residue. The mixture was then washed with water. Dichloromethane was distilled off from the dichloromethane layer. The remaining oil was purified by silica gel column chromatography to give the desired 3-(2-chloro-5-pyridylmethyl)-2-nitromethylenethiazolidine (1.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05428032 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-5a5eaaedd2d9437781fb424e6f14a887 |
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| 出典メモ | uspto-grants-1995_06 |
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