化工社化工社 化学情報印刷レポート · 研究参考用
Phenothiazine → Bis(trimethylsilyl)methylacrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | Bis(trimethylsilyl)chloromethane | HCID 552583 | — |
| 反応物 | Sodium acrylate | HCID 4068533 | — |
| 触媒 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 溶媒 | Butyronitrile | HCID 8008 | — |
| 生成物 | Bis(trimethylsilyl)methylacrylate | HCID 18764809 | — |
反応手順
Bis(trimethylsilyl)chloromethane (Aldrich) 39 g, 0.2 mole), sodium acrylate (28 g, 0.3 mole), Adogen 464 (Aldrich) (6.96 g), and phenothiazine (0.10 grams) were placed in a round bottom flask equipped with a condenser, mechanical stirrer and a nitrogen inlet. The flask was charged with 100 ml of butyronitrile and heated to reflux while stirring. After 6 hours, the mixture was diluted with 150 ml hexanes and filtered to remove the solids. The solvents were removed under reduced pressure. Fractional distillation of the residue under reduced pressure gave 35.5 grams 975%) of the desired product at 45-58° C. at 0.5 mm pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06653048B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-0e546afac53e4a3297d14375b599b8ea |
| 出典メモ | uspto-grants-2003_11 |