関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | (6-Chloropyridin-2-yl)methanol | HCID 182139 | — |
| 反応物 | Chloromethyl-2-(trimethylsilyl)ethyl ether | HCID 57232046 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-6-(2-(trimethylsilanyl)ethoxymethoxymethyl)pyridine | HCID 10802252 | 76.6% |
反応手順
3.20 ml of chloromethyl-2-(trimethylsilyl)ethyl ether (18.2 mmol) are added dropwise to a solution containing 2.50 g of (6-chloropyridin-2-yl)methanol (17.4 mmol), 3.30 ml of diisopropylethylamine (19.1 mmol) and 20 ml of dichloromethane cooled to 0° C. maintained under a nitrogen atmosphere. The mixture is stirred for 3 hours at room temperature and then the dichloromethane is evaporated off, the residue is taken up in water, the mixture is extracted with diethyl ether, the organic phase is washed with water and then dried over sodium sulfate. After filtration and evaporation of the solvent, the title product is isolated by chromatography on a silica column (eluent: dichloromethane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06020345 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-33e28e9b139c4391b28bbb1113071079 |
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| 出典メモ | uspto-grants-2000_02 |
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