関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 5-Fluoro-2-methylindan-1-one | HCID 3016257 | — |
| 反応物 | 4-Methylthiobenzyltriphenylphosphonium chloride | HCID 18969794 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 54074783 | HCID 54074783 | — |
反応手順
169 Mg. (1.5 mm) of potassium t-butoxide is dissolved in 2 ml. of DMSO and treated with 651 mg. (1.5 mm) of p-methylthiobenzyltriphenylphosphonium chloride dissolved in 1 ml. of DMSO. To this solution is added 270 mg. (1.65 mm) of 5-fluoro-2-methyl-1-indanone in 2 ml. of DMSO. The solution is heated at 75°C for 15.5 hours. Benzene and water are added and the benzene layer is washed five times with water. The benzene layer is dried over Na2SO4 and evaporated to dryness under vacuum. The weight is 915.6 mg. This material is eluted through 8 g. of silica gel with benzene to remove triphenylphosphine oxide. The eluate weights 372 mg. after removal of solvent. This is rechromatographed through 15 g. of silica gel using hexane and 95.9 mg. of 5-fluoro-2-methyl-1-(p-methylthiobenzylidene)-indane is isolated, melting point 67°-70°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US03944600 |
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| 出典データセット | uspto-grants-1976_03 |
|---|
| ORD ID | ord-2109a51794c743e4be107d5475ee5a84 |
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| 出典メモ | uspto-grants-1976_03 |
|---|
