関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | p-Methylcinnamoyl chloride | HCID 53411298 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 24186-38-7 | HCID 53914129 | — |
反応手順
3-p-Tolyl-acryloyl chloride (22.3 g, 123.3 mmol) in dioxane (50 mL) is slowly added to an ice cooled solution of sodium azide (16 g, 246.6 mmol) in water/dioxane (50 mL, 1/1, v/v) so as to maintain the temperature between 5-10° C. The mixture is stirred for 1.5 hours then poured over 300 g of ice. The resulting white solid is filtered and washed with additional water. The solid (20.72 g, 110.7 mmol) was dried over P2O5 under vacuum overnight and used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06281227B1 |
|---|
| 出典データセット | uspto-grants-2001_08 |
|---|
| ORD ID | ord-2cb7e8858e39471b9809495ab6419188 |
|---|
| 出典メモ | uspto-grants-2001_08 |
|---|
