関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene, 1-bromo-4-(trifluoromethyl)- | HCID 67872 | — |
| 反応物 | 1-Benzyl-4-piperazin-1-yl-phthalazine | HCID 6404023 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 25065679 | HCID 25065679 | 37% |
反応手順
To a solution of 1-benzyl-4-piperazin-1yl-phthalazine (100 mg, 0.329 mmol) in 1 mL THF is added 4-bromo-benzotrifluoride (99 mg, 0.443 mmol), potassium tert-butoxide (55.3 mg, 0.493 mmol), XPhos [2-(Dicyclohexylphosphino)-2′,4′,6′-tri-1-propyl-1′-1′-biphenyl] (15.7 mg, 0.033 mmol), and palladium (II) acetate (11 mg, 0.16 mmol) in a 2 dram screw-top vial. The vial is evacuated and flushed with argon. The reaction mixture was heated to 110° C. for 18 hrs. The mixture is then poured into water (50 mL), and the precipitate is isolated by filtration. The resulting solid is purified by flash chromatography on silica gel (10-70% EtOAc:heptanes) to provide the desired product as yellow crystals (54 mg, 37% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536168B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-a0263b0c12aa448d90f3cddfd3abef19 |
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| 出典メモ | uspto-grants-2013_09 |
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