참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Indole | HCID 798 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Propanone,3-bromo-1,1,1-trifluoro-, oxime | HCID 2782273 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 1,1,1-trifluoro-3-(1H-indol-3-yl)propan-2-one oxime | HCID 76549379 | 89.2% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07741361B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-b4ff9c053414483a8dc282ade2689add |
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| 출처 메모 | uspto-grants-2010_06 |
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