関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | 1-Heptanethiol | HCID 15422 | — |
| 反応物 | 5-Hexyn-1-ol | HCID 70234 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 7-Thia-tetradecan-5-ene-1-ol | HCID 53643999 | 30% |
反応手順
To 1.332 gr (10 mmol) of n-heptyl mercaptan and 981 mg (10 mmol) of 5-hexyn-1-ol dissolved in 25 ml of heptane under an argon atmosphere was added a few crystals of dibenzoyl peroxide. The reaction was stirred magnetically and heated to reflux for 18 hours. It was then cooled and poured into 25 ml of 10% sodium bicarbonate and extracted with 3×25 ml of ethyl acetate. The organic phases were combined and dried over sodium sulfate, filtered, and evaporated to yield a yellow oil. The oil was chromatographed on eight silica gel type GF preparative plates, using hexane-ethyl acetate (4:1) as developing solvent. Following removal of the band corresponding to product from the plates, the product was extracted from the silica with methanol, 684 mg (30% yield) of pure 7-thia-tetradecan-5-ene-1-ol was obtained as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05840508 |
|---|
| 出典データセット | uspto-grants-1998_11 |
|---|
| ORD ID | ord-1f0cc94f655e4e0da4f7dfd568e2cffc |
|---|
| 出典メモ | uspto-grants-1998_11 |
|---|