関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | Azide | HCID 33558 | — |
| 反応物 | HCID 178418348 | HCID 178418348 | — |
| 生成物 | HCID 178418411 | HCID 178418411 | 32% |
反応手順
A flask is charged with 5.0 g (27 mmole) of 1,2-dibromoethane, 3.8 g (58 mmole) of sodium azide, and 50 ml of DMF. The mixture is heated at 50° C. with stirring under argon overnight. The mixture is worked up as described above, except that the azide solution is not evaporated down totally. When about 30 ml of solution remains the mixture is treated with 45 ml of a 1.3M solution of MeLi (58 mmole) as above. After 3 hr the reaction is worked up as described above, and a yellow solid is obtained. Crystallization from ether/petroleum ether affords 1.23 g (32% yield) of an off-white solid, mp 64°-6° C. Mass spectra (FAB) Calc (M+H) 145.1201, Found 145.1220±0.0015.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05731301 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-1a927144cffe4757b1c0239ad6f9ed5a |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|
