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Hydrochloric Acid → Dimethyl 2-(3-fluoro-naphthacene-5,12-dionyl)-malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl malonate | HCID 7943 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Difluoronaphthacene-5,12-dione | HCID 20089834 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Dimethyl 2-(3-fluoro-naphthacene-5,12-dionyl)-malonate | HCID 20089823 | — |
反応手順
1 g (3.4 mmol) of 2,3-difluoro-naphthacene-5,12-dione, 0.94 g (6.8 mmol) of potassium carbonate, 0.89 g (6.8 mmol) of dimethyl malonate and 20 ml of DMSO are stirred at 50° C. for 22 hours. The mixture is poured onto dilute hydrochloric acid and extracted with THF/toluene. The organic phase is washed with water, dried over sodium sulfate and evaporated. The product is purified by chromatography over silica gel (mobile phase: 1% acetone/99% CH2Cl2); yield 1.25 g (91%); melting point 225°-230° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05112977 |
| 出典データセット | uspto-grants-1992_05 |
| ORD ID | ord-5ebc7f3d85fa45e2a39b1aade1d3c979 |
| 出典メモ | uspto-grants-1992_05 |