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Phosphorus oxychloride → 2-Chloro-4,5-diphenylpyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 5,6-Diphenyl-1-methyl-2(1H)-pyrimidinone | HCID 3609352 | — |
| 生成物 | 2-Chloro-4,5-diphenylpyrimidine | HCID 12674276 | — |
反応手順
A solution of 1-methyl-5,6-diphenyl-1H-pyrimidin-2-one (106, 314 mg, 1.20 mmol), phosphorus oxychloride (0.6 ml, 6.4 mmol) and phosphorus pentachloride (55 mg, 0.26 mmol) was heated at 120° C. for 3 hours. The excess amount of phosphorus oxychloride was removed under reduced pressure and cold water was added to the residue. The resulting precipitate was extracted with CH2Cl2. The organic layer was washed with brine, and dried over MgSO4, and concentrated in vacuo. The residue was purified by column chromatography (20% ethyl acetate in hexane) to produce the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728014B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-c92f9d8542fc4ac49029ecc678997a58 |
| 出典メモ | uspto-grants-2010_06 |