関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 生成物 | Morpholine-4-sulfonyl chloride | HCID 12798265 | — |
反応手順
With intensive cooling, 32.7 ml of sulfuryl chloride are added at approximately 0° C. to 23.5 ml of morpholine. The suspension is then carefully heated to 60° C., causing the onset of hydrogen chloride evolution. After 5 h at 60° C., the evolution of hydrogen chloride is complete. The cooled brown reaction mixture is poured onto ice, and the precipitating oil is extracted with ether, washed with water, 5% sodium hydrogen carbonate solution and water and dried with sodium sulfate. The organic phases are concentrated by evaporation and distilled at elevated temperature and reduced pressure (90° C.; 1 mbar) to yield the title compound: 1H-NMR (200 MHz, DMSO-d6): 3.80 and 3.29 (2t, 5 Hz, per 4 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05643878 |
|---|
| 出典データセット | uspto-grants-1997_07 |
|---|
| ORD ID | ord-11cbb57f44924c35a4f39d69eccf336a |
|---|
| 出典メモ | uspto-grants-1997_07 |
|---|