関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | Potassium cyclopropyltrifluoroborate | HCID 23697338 | — |
| 反応物 | 8-Chloro-2,2-dimethylchroman-6-carbaldehyde | HCID 77230856 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Cyclopropyl methyl ether | HCID 68323 | — |
| 生成物 | 8-Cyclopropyl-2,2-dimethylchroman-6-carbaldehyde | HCID 77230855 | — |
反応手順
A vial was charged with Pd(OAc)2 (7.99 mg, 0.04 mmol), XPhos (25.5 mg, 0.05 mmol), potassium carbonate (148 mg, 1.07 mmol), potassium cyclopropyltrifluoroborate (58.0 mg, 0.39 mmol) and 8-chloro-2,2-dimethyl-3,4-dihydro-2H-chromene-6-carbaldehyde (80 mg, 0.36 mmol). The mixture was dissolved in cyclopropylmethyl ether (1.62 mL) and water (0.16 mL) and purged with Ar. The reaction mixture was then stirred at 100° C. overnight, cooled to room temperature and filtered through a pad of celite. The filtrate was concentrated under vacuum, and the crude residue was purified by silica gel chromatography eluting with 0-20% EtOAc/hexanes to afford the desired product as a pale-yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08742110B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-1d789b5d164446f4ab2bade875d161c1 |
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| 出典メモ | uspto-grants-2014_06 |
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