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(Triphenylphosphoranylidene)acetaldehyde → 5,5-Bis(2-fluoro-4-methylphenyl)-4-(1-methyl-1H-tetrazol-5-yl)-2,4-pentadienal
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (Triphenylphosphoranylidene)acetaldehyde | HCID 75051 | — |
| 反応物 | 3,3-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)-2-propenal | HCID 14723994 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 5,5-Bis(2-fluoro-4-methylphenyl)-4-(1-methyl-1H-tetrazol-5-yl)-2,4-pentadienal | HCID 54207376 | 89.9% |
反応手順
A solution of 3,3-bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)-2-propenal (1.35 g, 3.8 mmoles) and triphenylphosphoranylidene acetaldehyde (1.16 g, 3.8 mmoles) in benzene was heated at reflux for 3 hours. The solvent was removed and the residue purified by column chromatography on silica gel eluting with 1% (v/v) methanol in methylene chloride. The fractions containing material having Rf =0.9 [methanol-methylene chloride; 1.20 (v/v)] were combined and concentrated to give 1.3 g of the title compound; m.p.=88°-108° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05068346 |
| 出典データセット | uspto-grants-1991_11 |
| ORD ID | ord-ab43328880904e13ae634977a4284a12 |
| 出典メモ | uspto-grants-1991_11 |