関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Ethyl chloroacetate | HCID 7751 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Diethyl 2-(benzyloxycarbonylamino)malonate | HCID 259787 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl 2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinate | HCID 66725114 | 86.1% |
反応手順
A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.27 g), and ethyl 2-chloroacetate (2.6 g) in DMF (50 mL) was stirred at 50° C. for 1 hour. The reaction mixture was cooled, and then poured into diluted hydrochloric acid, the mixture was extracted with ethyl acetate, and the extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from ethyl acetate/n-hexane to obtain the title compound (5.5 g, yield: 86%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434737B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-3894c10f70494b50b9b7b28ab01b5f7e |
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| 出典メモ | uspto-grants-2016_09 |
|---|
