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Potassium Carbonate → (2,3-Dihydro-1,4-benzoxathiin-2-yl)acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenol, o-mercapto-(6CI,7CI,8CI) | HCID 70718 | — |
| 反応物 | 3,4-Dibromobutanenitrile | HCID 11831139 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | (2,3-Dihydro-1,4-benzoxathiin-2-yl)acetonitrile | HCID 20540157 | — |
反応手順
The starting material is prepared as follows: To the stirred, refluxing solution of 21 g of 2-hydroxy-thiophenol in 290 ml of acetone is added dropwise 12.5 g of 3,4-dibromo-butyronitrile along with small portions of 15.8 g of anhydrous potassium carbonate. After 30 minutes, the double addition procedure with said amounts of dibromo compound and potassium carbonate is repeated, and after a further 30 minutes said procedure is repeated a third time. The mixture is then refluxed for 20 hours, cooled, filtered, the residual salts washed with acetone, and the filtrate evaporated. The residue is distilled (bulb to bulb), and the fraction boiling at 185°/0.5 mm Hg collected, to yield the 2-(1,4-benzoxathian-2-yl)-acetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04129655 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-3cf8bb51fd534efaaea82d7a6cc71de6 |
| 出典メモ | uspto-grants-1978_12 |