化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 178418853、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium fluoride | HCID 25953 | — |
| 反応物 | Azidotrimethylsilane | HCID 78378 | — |
| 反応物 | HCID 178418975 | HCID 178418975 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178418853 | HCID 178418853 | — |
反応手順
A solution of Intermediate 36 (196 g) and trimethylsilyl azide (283 ml, Tokyo Kasei Kogyo) in dimethylformamide (667 ml) was added with cesium fluoride (305 g, Wako Pure Chemical Industries) with stirring and stirred at 70° C. for 4 days. The reaction mixture was cooled to room temperature and then added twice with water in a volume of 2.75 l in total. This reaction mixture was stirred with ice cooling for 2 hours, and the deposited precipitates were collected by filtration. Then, the precipitates were washed with water to obtain a roughly purified product of the title compound (142 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094789B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-b811f8e37f91454ca9c82dfe2654d854 |
| 出典メモ | uspto-grants-2006_08 |