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Lithium Hydroxide → Diethyl 2-benzoylamino-2-(2-phenylsulfanylethyl)malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | ((2-Chloroethyl)thio)benzene | HCID 21702 | — |
| 反応物 | Diethyl benzamidomalonate | HCID 66790 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | Diethyl 2-benzoylamino-2-(2-phenylsulfanylethyl)malonate | HCID 18381758 | 17.8% |
反応手順
A solution comprised of sodium iodide (7.9 g, 52.7 mmol) and 2-chloroethyl phenyl sulfide (4.7 g, 27.2 mmol) in acetone (40 mL) was refluxed for 15 hours. The reaction mixture was cooled, diluted with ice water and extracted with ethyl acetate. The extract was concentrated and the residue was combined with N-methylpyrrolidone (20 mL), lithium hydroxide (1.6 g, 67 mmol) and diethyl 2-benzoylaminomalonate (5 g, 18 mmol). The mixture was stirred at ambient temperature of 15 hours and then poured into cold water. The product was extracted with ethyl acetate and purified by silica gel chromatography to provide diethyl 2-benzoylamino-2-(2-phenylsulfanylethyl)malonate (1.316 g, 3.2 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06492362B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-2d69693921f947ef9869edd189980690 |
| 出典メモ | uspto-grants-2002_12 |