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1,3-Dibromopropane → 1-(3-Bromopropoxy)-2-fluorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 反応物 | 2-Fluorophenol | HCID 9707 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(3-Bromopropoxy)-2-fluorobenzene | HCID 7172293 | 26.2% |
反応手順
To a solution of 2-fluorophenol (0.040 mL, 0.448 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.450 mL, 4.43 mmol) followed by Cs2CO3 (0.232 g, 0.713 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (4 mL) and extracted with DCM (8 mL). The organic layer was dried through a phase separator and concentrated under vacuum. The residue was taken up in DMSO and purified by preparatory HPLC (without TFA) to give the title compound (0.0274 g, 26.2%). EI-MS Rt (2.24 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08853404B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-75daea08891645c2b76ac5cb1a1e57d2 |
| 出典メモ | uspto-grants-2014_10 |