化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium Chloride → Bromo-9-(2-hydroxy-4-phenyl-butyl)-2-pyridin-4-yl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-(2-Phenylethyl)oxirane | HCID 135955 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 3-Bromo-2-pyridin-4-yl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one | HCID 136092380 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Bromo-9-(2-hydroxy-4-phenyl-butyl)-2-pyridin-4-yl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one | HCID 59796509 | — |
反応手順
A mixture of 3-Bromo-2-pyridin-4-yl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one (0.45 g, 1.46 mmol) and 2-Phenethyl-oxirane (0.65 g, 4.4 mmol) in DMF (20 mL) was treated LiHMDS (5 mL, 5 mml). The mixture was heated at 90 C for 1 h and was cooled to room temperature. Saturated NH4Cl (50 mL) was added and the mixture was extracted with CH2Cl2 (3×20 mL). The organic phase was washed with H2O (3×), dried (Na2SO4), and concentrated. The resulting brown oil was chromatographed on silica with 1-5% (2N NH3-MeOH)/CH2Cl2 to afford the product as a white solid. M+1 457.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429594B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-bbb7399147164b5c850f0512570b1803 |
| 出典メモ | uspto-grants-2008_09 |