化工社化工社 化学情報印刷レポート · 研究参考用
Triphenylphosphine → Methyl 3-chloro-4-(1,3-difluoropropan-2-yloxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 1,3-Difluoro-2-propanol | HCID 67985 | — |
| 反応物 | Methyl 3-chloro-4-hydroxybenzoate | HCID 77580 | — |
| 反応物 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 3-chloro-4-(1,3-difluoropropan-2-yloxy)benzoate | HCID 67248585 | 131.9% |
反応手順
To a solution of 1,3-difluoropropan-2-ol (2.57 g, 26.8 mmol) in THF (35 mL) was added methyl 3-chloro-4-hydroxybenzoate (2.00 g, 10.72 mmol), followed by triphenylphosphine (7.03 g, 26.8 mmol) and DIAD (5.21 mL, 26.8 mmol). The reaction was stirred overnight at room temperature, diluted with EtOAc and washed with brine. The organics were separated, washed with brine, dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography to give the title compound (3.743 g) as a clear oil. LCMS m/z=265.1 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108969B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-9ed069f600d349998924b808e3b82e77 |
| 出典メモ | uspto-grants-2015_08 |