化工社化工社 化学情報印刷レポート · 研究参考用
2-Bromoanisole → 2-(2'-Methoxy-[1,1'-biphenyl]-2-yl)-4,4-dimethyl-2-oxazoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromoanisole | HCID 11358 | — |
| 反応物 | 4,4-Dimethyl-2-(2-methoxyphenyl)oxazoline | HCID 333189 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | HCID 178489560 | HCID 178489560 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2'-Methoxy-[1,1'-biphenyl]-2-yl)-4,4-dimethyl-2-oxazoline | HCID 12611012 | 90% |
反応手順
2-Methoxyphenylmagnesium bromide, prepared from 2-bromoanisole (22.4 g, 120 mmol) and magnesium (2.9 g, 120 mmol), in dry THF (75 ml) was added dropwise to a stirred solution of 2-(2-methoxyphenyl)-4,4-dimethyl-2-oxazoline (20.4 g, 100 mmol) in dry THF (150 ml) under N2 at 20° C. Stirring of the solution was continued for 20 hours and then the reaction mixture was quenched by the addition of saturated ammonium chloride solution. The resulting mixture was extracted with ether (2×500 ml), dried over MgSO4, filtered and evaporated. The residue was chromatographed on silica gel (ethyl acetate-hexane) to provide title compound as colorless crystals (25.3 g, 90%), mp 129°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04375475 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-7aa77486be2f4976a415c984f8913fa5 |
| 出典メモ | uspto-grants-1983_03 |