関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2-Fluoro-4-hydroxybenzonitrile | HCID 2734675 | — |
| 反応物 | HCID 178447887 | HCID 178447887 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178447885 | HCID 178447885 | 67% |
反応手順
A suspension of 2.68 g of 4-[trans-4-(1E-propenyl)cyclohexyl]benzoic acid, 1.8 g of 4-cyano-3-fluorophenol and 187 mg of 4-(dimethylamino)pyridine in 25 ml of methylene chloride was cooled to 0° C. and treated while stirring with 3.17 g of N,N'-dicyclohexylcarbodiimide. After stirring at 0° C. for 5 minutes and at room temperature for 3 hours the suspension was filtered and the filtrate was concentrated. Chromatographic purification of the residue on 50 g of basic aluminium oxide with methylene chloride and subsequent crystallization from hexane/ethyl acetate gave 2.67 g of 4-cyano-3-fluorophenyl 4-[trans-4-(1E-propenyl)cyclohexyl]benzoate as colourless crystals; m.p. (C-N) 117.5° C., cl.p. (N--I) 233.1° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05413734 |
|---|
| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-16b0ae39a91848c6bc4715836e1e5cb1 |
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| 出典メモ | uspto-grants-1995_05 |
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