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Hydrochloric Acid → 1-((2-Benzoylphenylthio)methyl)cyclohexanecarboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Mercaptobenzophenone | HCID 3499713 | — |
| 反応物 | 1-(Mesyloxymethyl)cyclohexanecarboxaldehyde | HCID 22325261 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 1-((2-Benzoylphenylthio)methyl)cyclohexanecarboxaldehyde | HCID 22325208 | 75.9% |
反応手順
A mixture of 69 g (0.303 mole) of 2-mercaptobenzophenone, 82 g (0.303 mole) of mesylate 55, 32 g of triethylamine, and 150 ml of diglyme was stirred and held at reflux for 24 h. The mixture was cooled, poured into dil. HCl and extracted with methylene chloride. The organic layer was washed with 10% NaOH, water, brine, and dried over sodium sulfate and concentrated under vacuum to remove excess diglyme. This was purified by silica gel flush column (5% EtOAc:Hexane) and gave 18.6 g (75.9%) of yellow oil. Proton NMR and mass spectra were consistent with the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06420417B1 |
| 出典データセット | uspto-grants-2002_07 |
| ORD ID | ord-2f71fdaa36f94a28b4301990659889dc |
| 出典メモ | uspto-grants-2002_07 |