化工社化工社 化学情報印刷レポート · 研究参考用
Triethyl phosphonoacetate → HCID 67249397、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethyl phosphonoacetate | HCID 13345 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 7-Methoxy-8-methyl-2,3-dihydro-1H-pyrrolo[1,2-a]indol-1-one | HCID 67249703 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 67249397 | HCID 67249397 | 54.5% |
反応手順
To a solution of ethyl 2-(diethoxyphosphoryl)acetate (1.38 mL, 6.97 mmol) in DMF (2 mL) was added sodium hydride (60% dispersion in mineral oil) (279 mg, 6.97 mmol) at 0° C. The reaction mixture was stirred for 10 min, then 7-methoxy-8-methyl-2,3-dihydro-1H-pyrrolo[1,2-a]indol-1-one (500 mg, 2.323 mmol) in DMF (6 mL) was added. The reaction mixture was warmed to room temperature and stirred for 1 h, then heated at 60° C. for 1 h, cooled down, poured into saturated NH4Cl aqueous solution, extracted with ethyl acetate. The combined organics were washed with water, dried over anhydrous Na2SO4, and concentrated. The residue was purified by silica gel column chromatography to give the title compound (361 mg). LCMS m/z=286.2 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108969B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-eaaf330fbb24494b89c9cc983861df88 |
| 出典メモ | uspto-grants-2015_08 |