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Lithium Chloride → 4-Cyano-2-(2-phenylethynyl)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | Tris(furan-2-yl)phosphane | HCID 521585 | — |
| 反応物 | Tributyl(2-phenylethynyl)stannane | HCID 630640 | — |
| 反応物 | 4-Cyano-2-trifluoromethylsulphonylbenzaldehyde | HCID 54002071 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 4-Cyano-2-(2-phenylethynyl)benzaldehyde | HCID 54356802 | — |
反応手順
A mixture of 4-cyano-2-trifluoromethylsulphonyl-benzaldehyde (1.75 g, 6.3 mmol), tris(dibenzylidenacetone)dipalladium(o) (116 mg, 0.13 mmol), tris(2-furyl)phosphine (234 mg, 1.0 mmol) and anhydrous lithium chloride (0.8 g, 18.9 mmol) in dry N-methyl pyrrolidinone (18 ml) were reacted with (phenylethynyl)tri-n-butyltin (2.91 g, 7.4 mmol) for 3 hours at 50° C. and worked up following the procedure described in Example 15 (i). The crude oil was chromatographed on flash silica eluting with hexane-diethyl ether (4:1) to give 4-cyano-2-(2-phenylethynyl)benzaldehyde as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05863947 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-2fe22a9cfc544a6bbcdf55fe959a3660 |
| 出典メモ | uspto-grants-1999_01 |