化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 5-(((1-methyl-6-oxo-2,3,4,6-tetrahydro-1H-pyrimido[1,6-a]pyrimidin-8-yl)oxy)methyl)-2-(3-(trifluoromethyl)phenoxy)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-(Hydroxymethyl)-2-(3-(trifluoromethyl)phenoxy)benzonitrile | HCID 66825436 | — |
| 反応物 | 8-Chloro-1-methyl-3,4-dihydro-1H-pyrimido[1,6-A]pyrimidin-6(2H)-one | HCID 71743471 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(((1-methyl-6-oxo-2,3,4,6-tetrahydro-1H-pyrimido[1,6-a]pyrimidin-8-yl)oxy)methyl)-2-(3-(trifluoromethyl)phenoxy)benzonitrile | HCID 71236788 | 50.1% |
反応手順
To a solution of 8-chloro-1-methyl-3,4-dihydro-1H-pyrimido[1,6-a]pyrimidin-6(2H)-one (31 mg, 0.153 mmol) and 5-(hydroxymethyl)-2-(3-(trifluoromethyl)phenoxy)benzonitrile (49.4 mg, 0.168 mmol) in N, N-dimethylformamide (DMF) (1.5 mL), was added NaH (18.36 mg, 0.459 mmol). The reaction mixture was stirred at rt for 30 min. Aqueous HCl solution was added to adjust pH to ˜7. Purification by Mass Directed AutoPrep (MDAP) afforded the title compound as a white solid (35 mg, 50% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09273054B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-0c9e5201ecb743db9072ce8594cefd05 |
| 出典メモ | uspto-grants-2016_03 |