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Water → 6-Methoxy-1-[2-(4-trifluoromethyl-phenyl)-ethyl]-4,9-dihydro-3H-beta-carboline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | N-[2-(5-Methoxy-1H-indol-3-yl)-ethyl]-3-(4-trifluoromethyl-phenyl)-propionamide | HCID 59820000 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Methoxy-1-[2-(4-trifluoromethyl-phenyl)-ethyl]-4,9-dihydro-3H-beta-carboline | HCID 136207529 | 15.4% |
反応手順
A mixture of 0.61 g (1.57 mmol) N-[2-(5-methoxy-1H-indol-3-yl)-ethyl]-3-(4-trifluoromethyl-phenyl)-propionamide and 1 mL POCl3 in 2.5 mL acetonitrile was heated to reflux for 16 h. Water was added and the mixture was subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The combined product fractions were evaporated to dryness to yield 0.09 g (15%) of the title compound as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067598B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-7228d24817544f52bb660c76cfc051c3 |
| 出典メモ | uspto-grants-2011_11 |