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Ammonia → alpha-Amino-1,3-benzodioxole-5-acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Piperonal | HCID 8438 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | alpha-Amino-1,3-benzodioxole-5-acetonitrile | HCID 4405684 | — |
反応手順
Piperonal (6.00 g) is dissolved in THF (25 mL) and aq. NH3 (58%, 4.2 mL), NH4Cl (3.3 g) and KCN (3.9 g) are added. The mixture is stirred efficiently for 24 h. MgSO4 is added and the mixture stirred for 30 min., filtered and washed with THF. The filtrate is evaporated under reduced pressure and the residue purified by FC (Et2O/petrol ether 1:2,→2:1,→Et2O). Aminonitrile W-99 is obtained as a brown, unstable oil (2.87 g). The hydrochloride salt is precipitated from sat. HCl/Et2O for analytical purposes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06500842B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-2b2b0778e3e54a11be5f751f58d9a175 |
| 出典メモ | uspto-grants-2002_12 |