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Tetrahydrofuran → HCID 10341205、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 4-Bromo-2-chloroanisole | HCID 3016537 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 4-Tert-butyldimethysilyloxy-2-(3,4,5-trimethoxy-phenyl)-cyclopent-2-en-1-one | HCID 69110186 | — |
| 生成物 | HCID 10341205 | HCID 10341205 | — |
反応手順
A mixture of magnesium turnings (0.31 g, 13.1 mmol), 2-chloro-4-bromoanisole (3.00 g, 13.5 mmol), 4-tert-butyldimethysilyloxy-2-(3,4,5-trimethoxy-phenyl)-cyclopent-2-en-1-one (2.58 g, 6.84 mmol) and dry tetrahydrofuran (35 ml) under nitrogen was stirred at room temperature for 4 h. Reaction was then quenched with dil hydrochloric acid (30 ml), tetrahydrofuran was removed under reduced pressure and the residual reaction mixture was extracted with ethyl acetate (3×35 ml), washed with water (2×20 ml) and dried over sodium sulfate. Concentration and purification by column chromatography over silica gel (eluent-6% acetone in pet ether) afforded the alcohol of the formula (4A)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179937B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-a9576572c5124dd0afedcff1b018c3f3 |
| 出典メモ | uspto-grants-2007_02 |