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Acetic Anhydride → 5-Methyl-4-(1-acetoxytridecyl)-2-trimethylsilylfuran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 1-Bromododecane | HCID 8919 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 5Methyl-2-trimethylsilyl-4-furaldehyde | HCID 15744590 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Methyl-4-(1-acetoxytridecyl)-2-trimethylsilylfuran | HCID 19433185 | — |
反応手順
A mixture of 1-bromododecane (261 mg, 0.11 mmol) and magnesium turnings (27 mg, 0.11 mmol) in tetrahydrofuran (7 ml) was refluxed under argon for 1 hour. After cooling to room temperature, a solution of 5-methyl-2-trimethylsilyl-4-furaldehyde (158.6 mg, 0.87 mmol) in tetrahydrofuran (1 ml) was added, followed by acetic anhydride (0.25 ml, 2.6 mmol) after 1 hour. Stirring was continued at room temperature overnight and the mixture was quenched with water. Extraction (ethyl ether) and evaporation of the dried (magnesium sulphate) extracts gave an oil, which was purified by preparative TLC (20×20 cm, 1000 micron silica plate; developed with 5% ethyl ether/hexane). The title ester was obtained as a light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05298633 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-dca08df96bca4e8999c4587933fcfd3a |
| 出典メモ | uspto-grants-1994_03 |