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Rac-2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxy-5-pyridin-2-ylmethylcyclopent-2-enone → HCID 89600897、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Rac-2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxy-5-pyridin-2-ylmethylcyclopent-2-enone | HCID 89600971 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | HCID 89600897 | HCID 89600897 | — |
反応手順
A solution of rac-2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxy-5-pyridin-2-ylmethylcyclopent-2-enone (0.5 g, 1.45 mmol) in acetone (10 ml) and 2N hydrochloric acid (5 ml) is heated at 80°C. under microwave irradiation for 40 minutes. Volatile solvents are removed in vacuo and residue is diluted with distilled water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organic fractions are washed again with distilled water, brine, dried over sodium sulfate, filtered and the filtrate concentrated in vacuo. The crude product is purified by flash column chromatography to afford rac-2-(2,6-Dimethyl-4-prop-1-ynylphenyl)-4-pyridin-2-ylmethylcyclopentane-1,3-dione.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09107415B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-ac0e587f98fc4228b286f8fcc785b8aa |
| 出典メモ | uspto-grants-2015_08 |