関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dichloro-5-(chloromethyl)pyridine | HCID 10176536 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,3-Dichloro-5-(methoxymethyl)pyridine | HCID 11137960 | — |
反応手順
Under argon and at room temperature, 4.14 g (23 mmol) of sodium methoxide (30 percent strength solution in methanol) was added dropwise within 5 minutes to a solution of 4.11 g (20.9 mmol) of 2,3-dichloro-5-(chloromethyl)-pyridine [prepared from 2,3-dichloro-5-(hydroxymethyl)-pyridine by reaction with thionyl chloride] in 40 ml of methanol. The reaction mixture was subsequently heated to 60° C. for 3 hours. After the reaction had ended, the solvent was distilled off and the residue was admixed with 100 ml of water and extracted with dichloromethane (3×75 ml). The organic phase was dried over magnesium sulfate and evaporated. The yield of the product was 4.06 g (90.4 percent) of a yellow oil, purity (GC) 90.8 percent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05925765 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-417f070d4f034bef938334c2140ee6ab |
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| 出典メモ | uspto-grants-1999_07 |
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