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Triphenylphosphine → 3-[2-(2-Fluoro-5-methyl-phenyl)-ethoxy]-4-methoxy-benzoic Acid Methyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Methyl 3-hydroxy-4-methoxybenzoate | HCID 4056967 | — |
| 反応物 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 反応物 | 2-(2-Fluoro-5-methyl-phenyl)-ethanol | HCID 58318372 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-[2-(2-Fluoro-5-methyl-phenyl)-ethoxy]-4-methoxy-benzoic Acid Methyl Ester | HCID 67170456 | 60.5% |
反応手順
2-(2-Fluoro-5-methyl-phenyl)-ethanol (508 mg, 3.29 mmol) was dissolved in THF (23 ml). Triphenylphosphine (1.08 g, 4.12 mmol) and 3-hydroxy-4-methoxy-benzoic acid methyl ester (500 mg, 2.75 mmol) were added, the mixture was cooled in an ice bath, and DIAD (832 mg, 4.12 mmol) was added slowly with stirring. The ice bath was removed and stirring was continued overnight at room temperature. The volatiles were evaporated in vacuo, and the residue was purified by RP HPLC (water/ACN gradient) to give 530 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618304B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-a18d6fa229bf42acaf4f2ef904d1fcb7 |
| 出典メモ | uspto-grants-2013_12 |