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1,3-Propanediol → 2-(4-Nitrobenzyl)-1,3,2-dioxaphosphinane 2-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Propanediol | HCID 10442 | — |
| 反応物 | (4-Nitrobenzyl)phosphonic dichloride | HCID 10377593 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Nitrobenzyl)-1,3,2-dioxaphosphinane 2-oxide | HCID 11345893 | — |
反応手順
Crude (4-Nitrobenzyl)phosphonic dichloride (Compound 230E) above was dissolved in anhydrous THF (20 mL). To this solution was added TEA (840 mg, 7.5 mmol) and 1,3-propane-diol (190 mg, 2.5 mmol) at 0° C. The resulting mixture was stirred at room temperature overnight, concentrated and the residue was purified by column chromatography to give the target product (70 mg). 1H NMR (CD3OD, 400 MHz): δ=2.85 (d, J=20.0 Hz, 2H), 3.28-3.30 (m, 2 H), 3.55-3.58 (m, 2 H), 3.75-7.78 (m, 2 H), 6.64 (d, J=8.4 Hz, 2 H), 7.07 (d, J=8.4 Hz, 2 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09096624B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-03861766c05243e2b77bbea746306971 |
| 出典メモ | uspto-grants-2015_08 |