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Acetone → Nonane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 反応物 | 2,3,2'-Trifluoro-4-iodo-4''-propyl-[1,1';4',1'']-terphenyl | HCID 11247963 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Nonane | HCID 8141 | 68% |
反応手順
A solution of (0.1 mmol) of 10, (0.12 mmol) of 14, 14 mg (0.13 mmol) of neopentyl glycol, 95 mg (0.3 mmol) of Ba(OH)2.8H2O, 80 μl (6.08 mmol, 5 mol %) of a 76 mM acetone solution of Pd(OAc)2 in 2 ml of 95% i-PrOH is stirred at 80° C. for 12 hours. The solvent is subsequently removed under reduced pressure. 2 ml of 2 M HCl are added to the residue, and the mixture is extracted with dichloromethane (3×2 ml). The combined organic phases are dried over MgSO4 and filtered through SiO2. The solvent is removed under reduced pressure, and the residue is purified by recrystallisation twice from nonane (yield: 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07183447B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-562e7b61b5e8420ead91f8ba71d0fdfd |
| 出典メモ | uspto-grants-2007_02 |