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Methanol → 1-Benzyl-2-methyl-5-(2,4-difluorophenyl)-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,4-Difluorophenylboronic acid | HCID 2734334 | — |
| 反応物 | 1-Benzyl-2-methyl-5-bromo-1H-imidazole | HCID 66868795 | — |
| 触媒 | Palladium(2+) acetate--triphenylphosphane (1/2/2) | HCID 84538 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 1-Benzyl-2-methyl-5-(2,4-difluorophenyl)-1H-imidazole | HCID 66869085 | 67.5% |
反応手順
Heat a mixture of 1-benzyl-2-methyl-5-bromo-1H-imidazole (4.71 g, 18.7 mmol), 2,4-difluorophenyl boronic acid (6.92 g, 43.8 mmol), bis(acetato)bis(triphenylphosphine)-palladium(II) (1.4 g, 1.875 mmol), 2N Na2CO3 (19 mL, 38 mmol), MeOH (19 mL) and 1,2-dimethoxyethane (120 mL) to reflux for 18 h. Cool to RT. Add water and EtOAc and separate the layers. Dry organic layer over MgSO4, filter, and concentrate. Purify the residue (silica gel chromatography, eluting with EtOAc:CH2Cl2 mixtures) to give the desired compound (3.59 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07582652B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-663562bcc74b4a6da309af86daf84192 |
| 出典メモ | uspto-grants-2009_09 |