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Hydrogen Cyanide → 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Cyanide | HCID 768 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2H-1,5-Benzodioxepin-3(4H)-one | HCID 11309700 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin | HCID 15557293 | — |
反応手順
To a stirred solution of 4.92 g. (30 millimoles) of 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin in 100 mls. of benzene is added dropwise a solution of 30 millimoles of anhydrous hydrogen cyanide in 50 ml. of benzene. The reaction mixture is stirred overnight at ambient temperature, basified with 10% sodium carbonate solution and the organic layer separated. The benzene solution is washed once with water and dried successively over anhydrous magnesium sulfate and calcium sulfate. Evaporation of the solvent under reduced pressure at 40° C. yields the crude cyanohydrin which upon purification and mixed melting point determination gives no depression with an authentic sample of 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03944560 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-e6799d215004407bbdec444fa4284f11 |
| 出典メモ | uspto-grants-1976_03 |