関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Silane, (chloromethyl)trimethyl- | HCID 75361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Trimethylsilanylmethoxybenzaldehyde | HCID 56528964 | 84% |
反応手順
Chloromethyltrimethylsilane (110.5 g, 0.9 mol) is added dropwise over 30 minutes to a mixture of para-hydroxybenzaldehyde (110 g, 0.82 mol) and potassium carbonate (124.5 g, 0.9 mol) in 1 L of dry DMF maintained at 80° C., and while sparging with nitrogen. The mixture is left at 90° C. for 4 hours. The reaction mixture is filtered and the solvent is removed from the filtrate by distillation under vacuum. The final traces of DMF are removed via a stage at 60° C. under a vacuum of 2 mmHg. 142.4 g (yield: 84%) of 4-trimethylsilanylmethoxybenzaldehyde are obtained in the form of an orange-yellow oil, which is used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07354571B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-dfab117446f04b698ae0f92944dbd878 |
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| 出典メモ | uspto-grants-2008_04 |
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