関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Vanillin | HCID 1183 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (3-Chloropropyl)trimethylsilane | HCID 75362 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Methoxy4-(3-trimethylsilanylpropyloxy)benzaldehyde | HCID 18463172 | 89.1% |
反応手順
3-chloropropyltrimethylsilane (33.14 g, 0.22 mol) was added dropwise over 20 minutes to a mixture of vanillin (30.4 g, 0.2 mol) and potassium carbonate (30.4 g, 0.22 mol) in 150 ml of dry DMF heated to 80° C. under nitrogen. The mixture was maintained for 4 hours at 95°-110° C. The reaction mixture was cooled and poured into ice-cold water. The aqueous phase was extracted three times with dichloromethane. The organic phases were dried over sodium sulfate and concentrated under vacuum. After distillation under vacuum (0.04 mm Hg), 47.5 g (yield: 89%) of 3-methoxy-4-(3-trimethylsilanylpropyloxy) benzaldehyde were obtained in the form of a slightly pinkish oil distilling at 112°-114° C. and employed without further purification in the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06429326B1 |
|---|
| 出典データセット | uspto-grants-2002_08 |
|---|
| ORD ID | ord-bfc65781d7b8491b8a3844521f286065 |
|---|
| 出典メモ | uspto-grants-2002_08 |
|---|