関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(chloromethyl)-1,3-dimethoxyBenzene | HCID 12707002 | — |
| 反応物 | 1-(4-Chloro-6-methyl-2-pyridinyl)ethanone oxime | HCID 136388351 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Chloro-6-methyl-2-pyridinyl)ethanone O-[(2,6-Dimethoxyphenyl)methyl] Oxime | HCID 73178432 | — |
反応手順
On the other hand, 1.66 g (9.0 mmol) of 1-(4-chloro-6-methyl-2-pyridinyl)ethanone oxime was dissolved in 15 ml of N,N-dimethylformamide, and the resultant solution was added with 0.18 g (4.39 mmol) of sodium hydride (60%, oiliness) while cooling the solution with ice. The mixture was stirred for 15 min. at a temperature below 0° C. and was added with the whole amount of the crude product of 2,6-dimethoxybenzyl chloride prepared previously while cooling the mixture with ice. The resultant mixture was stirred for 2.3 hours at a room temperature to complete a reaction. The reacted mixture was then poured into ice water. At that time, the target compound was precipitated in the ice water. The precipitation was taken out by filtering, washed with hexane and dried to thereby obtain the target compound in an amount of 2.3 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06589967B1 |
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| 出典データセット | uspto-grants-2003_07 |
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| ORD ID | ord-55117f21121146beabd2e6f74c49a34b |
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| 出典メモ | uspto-grants-2003_07 |
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