化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → [4-(2-Azepan-1-yl-ethoxy)-phenyl]-[6-methoxy-2-(2,4,6-trifluoro phenyl)-naphthalen-1-yl]-methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 2,4,6-Trifluorophenylboronic Acid | HCID 2779329 | — |
| 反応物 | Trifluoromethanesulfonic acid 1-[4-(2-azepan-1-yl-ethoxy)-benzoyl]-6-methoxynaphthalen-2-yl ester | HCID 57552509 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [4-(2-Azepan-1-yl-ethoxy)-phenyl]-[6-methoxy-2-(2,4,6-trifluoro phenyl)-naphthalen-1-yl]-methanone | HCID 57552563 | 35% |
反応条件
| 温度 | 100 °C |
|---|
反応手順
Dissolve trifluoromethanesulfonic acid 1-[4-(2-azepan-1-yl-ethoxy)-benzoyl]-6-methoxynaphthalen-2-yl ester (990 mg, 1.8 mmol), 2,4,6-trifluorophenylboronic acid (634 mg, 3.6 mmol), potassium phosphate (2.2 g, 10.8 mmol), tetrakis(triphenylphosphine)palladium (416 rag, 0.4 mmol) in dry DMF (25 mL) and heat at 100° C. for 3 hours. Purify reaction by SCX column. Additional purification is done by silica get chromatography using a 1-3% gradient of methanol in dichloromethane to yield 320 mg (35%) of the title compound: mass spectrum (ion spray) m/z=534 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08217032B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-260bfa4b6f724fd594f6cfffc770d153 |
| 出典メモ | uspto-grants-2012_07 |