関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 1-(Chloromethyl)-3,5-bis(trifluoromethyl)benzene | HCID 123576 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(Azidomethyl)-3,5-bis(trifluoromethyl)benzene | HCID 44185743 | — |
反応手順
Sodium azide (74.3 g, 1.14 mol) is suspended in water (125 mL), then DMSO (625 mL) is added. After stirring for 30 minutes, a solution consisting of 3,5-Bis(trifluoromethyl)benzyl chloride (255.3 g, 0.97 moles) and DMSO (500 mL) is added over 30 minutes. (The 3,5-Bis(trifluoromethyl)benzyl chloride is heated to 35° C. to liquefy prior to dispensing (MP=30-32° C.)). The benzyl chloride feed vessel is rinsed with DMSO (50 mL) into the sodium azide solution, the mixture is heated to 40° C., and then maintained for an hour at 40° C., then cooled to 23° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08772496B2 |
|---|
| 出典データセット | uspto-grants-2014_07 |
|---|
| ORD ID | ord-ac037c254dfd47ffaab08cedc7a253c6 |
|---|
| 出典メモ | uspto-grants-2014_07 |
|---|
