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2(1H)-Pyrimidinone, tetrahydro- → HCID 59586732、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2(1H)-Pyrimidinone, tetrahydro- | HCID 74615 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 1-Fluoro-2-isopropyl-4-nitrobenzene | HCID 59860488 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 59586732 | HCID 59586732 | — |
反応手順
347 mg (3.47 mmol) of tetrahydropyrimidinone in 21 ml of DMSO are admixed at RT with 584 mg (5.21 mmol) of potassium tert-butoxide, and the mixture is stirred at RT for 45 min. 700 mg (3.82 mmol) of 1-fluoro-2-isopropyl-4-nitrobenzene are added and the mixture is stirred at 60° C. After 18 h, it is cooled and diluted with 250 ml of water. It is extracted three times with ethyl acetate and the combined organic phases are dried over sodium sulfate. After filtration, the solvents are removed under reduced pressure and the residue is purified by chromatography on silica gel (1:5→1:10 cyclohexane/ethyl acetate). This affords 140 mg (14% of theory) of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198267B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-8a186f2eb15b422db9d30e34aaf3fc64 |
| 出典メモ | uspto-grants-2012_06 |