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Dimethylformamide → 1,2,3,4-Tetrahydro-2-[5-(3,4-dimethoxyphenyl)-pyrimidin-2-yl]-3-(3,4-methylenedioxyphenyl)-9H-pyrrolo-[3,4-b]quinolin-9-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Benzo[1,3]dioxol-5-yl-2-[5-(3,4-dimethoxy-phenyl)-pyrimidin-2-yl]-2,3,4,9-tetrahydro-1H-beta-carboline | HCID 11049430 | — |
| 生成物 | 1,2,3,4-Tetrahydro-2-[5-(3,4-dimethoxyphenyl)-pyrimidin-2-yl]-3-(3,4-methylenedioxyphenyl)-9H-pyrrolo-[3,4-b]quinolin-9-one | HCID 10301622 | — |
反応手順
Sodium hydride (60% in mineral oil, 40 mg, 1.0 mmol) and 1-(3,4-methylenedioxyphenyl)-2-[5-(3,4-dimethoxyphenyl)-pyrimidin-2-yl]-2,3,4,9-tetrahydro-1H-β-carboline (218 mg, 0.43 mmol) (prepared as in Example 13) in DMF (10 mL, anhydrous) were stirred at room temperature for 30 min. Dry air was then bubbled through the solution for 16 h. Ethyl acetate (100 mL) and saturated NaHCO3 were added, the organic phase was washed with water, brine, and dried with MgSO4. Solvent was evaporated and the residue purified by chromatography (silica gel, ethyl acetate) to yield the product as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06635638B2 |
| 出典データセット | uspto-grants-2003_10 |
| ORD ID | ord-37f5c5b3f8044fb889ae2eaff6ac1f79 |
| 出典メモ | uspto-grants-2003_10 |