関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Indole | HCID 798 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Propanone,3-bromo-1,1,1-trifluoro-, oxime | HCID 2782273 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 1,1,1-trifluoro-3-(1H-indol-3-yl)propan-2-one oxime | HCID 76549379 | 89.2% |
反応手順
To a solution of the 1.64 g (7.96 mmol) of 3-bromo-1,1,1-trifluoropropan-2-one oxime in 250 mL of methyl tert-butyl ether was added 3.74 g (31.92 mmol) of indole followed by 5.0 g (47.62 mmol) of powdered (freshly ground) sodium carbonate. The reaction was monitored by thin layer chromatography (ethyl acetate-hexanes (2:8)) to afford a new more polar product compared to indole (PMA-stained and UV-active). The mixture was then filtered through diatomaceous earth and concentrated in vacuo. The residue was then concentrated in vacuo and diluted first with dichloromethane (1 part) and then hexanes (4 parts) and passed through a pad of silica gel using dichloromethane-hexanes (gradient: 20%-100%) to afford 1.72 g (89.2%) of 1,1,1-trifluoro-3-(1H-indol-3-yl)propan-2-one oxime as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741361B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b4ff9c053414483a8dc282ade2689add |
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| 出典メモ | uspto-grants-2010_06 |
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