化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → (2-Nitro-phenylethynyl)-phosphonic acid diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | o-Iodonitrobenzene | HCID 69115 | — |
| 反応物 | Diethyl ethynylphosphonate | HCID 2784295 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (2-Nitro-phenylethynyl)-phosphonic acid diethyl ester | HCID 86638334 | — |
反応手順
To a solution of 300 mg of ethynyl-phosphonic acid diethyl ester, 494 mg of 1-iodo-2-nitrobenzene and 0.28 ml of di-isopropylamine in 15 ml THF are sequentially added 43 mg of bis-(triphenylphosphin)-palladium(II)-dichloride and 12 mg of copper(I)iodide and the mixture obtained is refluxed for approximately 2 hours. Following an acidic work-up (1N aqueous HCl and EtOAc) and subsequent column chromatography (2-nitro-phenylethynyl)-phosphonic acid diethyl ester is obtained in the form of a slightly brownish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08119617B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-f2dd420978b5476eb0aa2aceba494056 |
| 出典メモ | uspto-grants-2012_02 |