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Acetic Acid → 2-[4-(Trimethylsilanylmethoxy)benzylidene]malonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Malonamide | HCID 7911 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Trimethylsilanylmethoxybenzaldehyde | HCID 56528964 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-[4-(Trimethylsilanylmethoxy)benzylidene]malonamide | HCID 10108399 | 49% |
反応手順
4-(Trimethylsilanylmethoxy)benzaldehyde (obtained in step 1 of Example 1) (10.4 g, 0.005 mol) and malonamide (5.5 g, 0.055 mol) in 20 ml of dry toluene in the presence of 0.5 ml of piperidine and 0.3 g of acetic acid are refluxed for 3 hours in a reactor equipped with Dean-Stark apparatus. The water formed is removed azeotropically. The mixture is cooled and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and filtered, and the solvent is evaporated off under vacuum. After recrystallization from ethanol, 7.2 g (yield: 49%) of the derivative of Example 10 are obtained in the form of an off-white powder:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07354571B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-cc4c636fed4448b8bbc95fc511865ee1 |
| 出典メモ | uspto-grants-2008_04 |