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Phosphorus oxychloride → 1-[1-(4-Chlorophenyl)cyclobutyl]-7-methoxy-3,4-dihydroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1-(4-Chlorophenyl)-N-[2-(4-methoxyphenyl)ethyl]cyclobutanecarboxamide | HCID 60409722 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[1-(4-Chlorophenyl)cyclobutyl]-7-methoxy-3,4-dihydroisoquinoline | HCID 66868699 | — |
反応手順
1-(4-Chlorophenyl)-N-[2-(4-methoxyphenyl)ethyl]cyclobutanecarboxamide (10.58 g, 30.8 mmol) was treated with toluene (100 mL). Phosphoryl trichloride (4.72 g, 30.8 mmol) was added and the reaction mixture was heated under reflux for 8 h. After cooling to room temperature the reaction mixture was concentrated in vacuo and then slowly poured in ice water. Ethyl acetate was added and the organic layer was washed with water (2×), dried (MgSO4) and concetrated in vacuo to give an orange oil. Yield: 10.25 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653100B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-4f76c4855d6246aca806863959e6bead |
| 出典メモ | uspto-grants-2014_02 |