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Hydrochloric Acid → 2-((2-Benzoylphenylthio)methyl)-2-ethylhexanal
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 | 2-Ethyl-2-(mesyloxymethyl)hexanal | HCID 11572217 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 2-((2-Benzoylphenylthio)methyl)-2-ethylhexanal | HCID 11602826 | 58% |
反応手順
A mixture of 31 g (0.144 mol) of 2-mercaptobenzophenone, prepared according to the procedure described in WO 93/16055, 24.4 g (0.1 mole) of 2-ethyl-2-(mesyloxymethyl)-hexanal (1), 14.8 g (0.146 mole) of triethylamine, and 80 mL of 2-methoxyethyl ether was held at reflux for 24 h. The reaction mixture was poured into 3N HCl and extracted with 300 mL of methylene chloride, The methylene chloride layer was washed with 300 mL of 10% NaOH, dried over MgSO4 and concentrated in vacuo to remove 2-methoxyethyl ether. The residue was purified by HPLC (10% EtOAc-hexane) to give 20.5 g (58%) of 2 as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06642268B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-3ba2a7f111dd4316b2eab3ac37c46b53 |
| 出典メモ | uspto-grants-2003_11 |