関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Diethoxymethane | HCID 10024 | — |
| 反応物 | Allyl isocyanate | HCID 15123 | — |
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | N-allyl-3-trimethylsilylpropiolic amide | HCID 11217610 | — |
反応手順
The reaction is carried out by dissolving trimethylsilylacetylene in an solvent. Preferred solvents include ethereals such as THF, diethoxymethane and t-butylmethyl ether. At about 0° C., a strong base is added dropwise over a period of about 15 minutes. Examples of strong bases are n-butyl lithium and lithium diisopropyl amide. While still maintaining the temperature near 0° C., a solution of allyl isocyanate in solvent is added dropwise over about 15 minutes. This is followed by the dropwise addition of trimethylsilyl chloride. After holding the reaction mixture at about 0 to about 10° C. for about 3 hours, the reaction is quenched with aqueous ammonium chloride and extracted with dichloromethane. The solvent is evaporated to yield the product, N-allyl-3-trimethylsilylpropiolic amide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06291513B1 |
|---|
| 出典データセット | uspto-grants-2001_09 |
|---|
| ORD ID | ord-a31367e9ef604a1bad0292483a4caf64 |
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| 出典メモ | uspto-grants-2001_09 |
|---|
