関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | (E)-methyl 4-(dimethylamino)but-2-enoate | HCID 15870798 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (2E)-4-(Dimethylamino)-2-butenoic acid hydrochloride | HCID 45358758 | 51% |
反応手順
Methyl (2E)-4-(dimethylamino)but-2-enoate (3.4 g, 23.7 mmol) was dissolved in methanol (25 mL). A solution of sodium hydroxide (0.95 g, 23.7 mmol) in water (7 mL) was added, and the mixture was heated to 50° C. for 1 h. The pH was then adjusted to 2 with conc. hydrochloric acid. The solution was concentrated to dryness, and the residue was triturated with ethanol (30 mL). It was filtered, and the solution was concentrated in vacuo. The residue was triturated with 2-propanol, and the precipitate was collected by suction filtration and dried to yield 2.00 g (51%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524722B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-8dd1568111f34f96ba6ac11b4e5efd23 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|