関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dimethoxy-2-butyne | HCID 542354 | — |
| 反応物 | 2,2,2-trifluoro-N-[1-(2-propynyl)-3-butynyl]acetamide | HCID 22499180 | — |
| 触媒 | Chlorotris(triphenylphosphine)rhodium(I) | HCID 84599 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(Trifluoroacetylamino)-5,6-bis(methoxymethyl)indane | HCID 22499220 | — |
反応手順
According to the procedure of Magnus et. al (Tetrahed. Lett., 34, 23-26 (1993)) a solution of commercially available 1,4-dimethoxy-2-butyne (1.32 g, 11.5 mmol) in nitrogen-degassed ethanol is heated to 80° C. with stirring under a nitrogen atmosphere. Tris(triphenylphosphine)rhodium chloride (64 mg, 0.07 mmol) and a solution of 2,2,2-trifluoro-N-[1-(2-propynyl)-3-butynyl]-acetamide (470 mg, 2.32 mmol; prepared from literature procedure: Romero, Arthur G.; Leiby, Jeffrey A PCT Int. Appl. WO 9623760) in nitrogen-degassed ethanol (2 ml) are added in portions over 2 hours. The mixture is stirred under nitrogen at 80° C. for a further 3 hours. The solvent is removed under vacuo and the residue is purified by flash chromatography on silica gel, eluting with hexane/ethyl acetate (2:1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08283362B2 |
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| 出典データセット | uspto-grants-2012_10 |
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| ORD ID | ord-722856e3043c43069d8172b86711bcbe |
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| 出典メモ | uspto-grants-2012_10 |
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