化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Iodide → Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 反応物 | Potassium di-tert-butyl phosphate | HCID 23674467 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoate | HCID 90087888 | — |
反応手順
Methyl 4-(bromomethyl)benzoate (1200 mg, 5.24 mmol), potassium di-tert-butyl phosphate (1431 mg, 5.76 mmol) and sodium iodide (785 mg, 5.24 mmol) were combined in DMF (3.00 mL) under nitrogen. The reaction mixture was stirred at room temperature for 24 h. The reaction mixture was diluted with ether, washed with 10% LiCl solution and brine, then dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (hexane/EtOAc) to provide Preparation 55A (571 mg, 1.593 mmol, 30%): 1H NMR (400 MHz, CDCl3) δ 8.03 (d, J=8.4 Hz, 2H), 7.53-7.37 (m, 2H), 5.05 (d, J=7.5 Hz, 2H), 3.92 (s, 3H), 1.48 (d, J=0.4 Hz, 18H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09242941B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-ddb14697f5774d0e8ba27545822bb64b |
| 出典メモ | uspto-grants-2016_01 |