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3-(Chloromethyl)pyridine → 3-(3-Pyridylmethyl)2-nitromethylenethiazolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(Chloromethyl)pyridine | HCID 18358 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Nitromethylene-thiazolidine | HCID 3835583 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(3-Pyridylmethyl)2-nitromethylenethiazolidine | HCID 54251207 | 10.6% |
反応手順
2-Nitromethylenethiazolidine (2.9 g) was suspended in dry acetonitrile (30 ml), and 60% sodium hydride (0.9 g) was added under a nitrogen stream. Then, the mixture was stirred at room temperature until the generation of hydrogen ceased. A solution of 3-picolyl chloride (3.2 g) in dry acetonitrile (5 ml) was added, and the mixture was stirred at room temperature for 3 hours. Acetonitrile was distilled off under reduced pressure. Dichloromethane was added to the residue, and the mixture was washed with water. Dichloromethane was then distilled off from the dichloromethane layer. The remaining oily product was purified by column chromatography to give the desired 3-(3-pyridylmethyl)2-nitromethylenethiazolidine (0.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05428032 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-317d85161bc84df29e7177f6451668d2 |
| 出典メモ | uspto-grants-1995_06 |