関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4,5-Dimethoxy-1-indanone | HCID 240446 | — |
| 反応物 | 4-[(Trifluoromethyl)sulfanyl]benzaldehyde | HCID 2777846 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (E)-4,5-dimethoxy-2-(4-((trifluoromethyl)thio)benzylidene)-2,3-dihydro-1H-inden-1-one | HCID 117940284 | — |
反応手順
To a solution of 4,5-dimethoxy-2,3-dihydro-1H-inden-1-one (165) (100 mg, 0.520 mmol) in toluene 15 mL was added 4-((trifluoromethyl)thio)benzaldehyde (72) (118.4 mg, 0.572 mmol) and PTSA (178.9 mg, 1.414 mmol). The reaction was stirred at 120° C. for 6 h. The resulting reaction mixture was diluted with ethyl acetate and washed with water (3×25 mL). The organic layer was dried over sodium sulphate and concentrated to get the crude, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound was eluted at 25% ethyl acetate in hexane to afford yellow coloured solid of (E)-4,5-dimethoxy-2-(4-((trifluoromethyl)thio)benzylidene)-2,3-dihydro-1H-inden-1-one intermediate 166.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09359315B2 |
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| 出典データセット | uspto-grants-2016_06 |
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| ORD ID | ord-d8754f6256774591989d11c928876ce9 |
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| 出典メモ | uspto-grants-2016_06 |
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