関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 3-Phenoxy-1-phenylpropan-1-one | HCID 3876355 | — |
| 反応物 | Diethyl (1,3-Dithian-2-yl)phosphonate | HCID 10869064 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-{1-(4-Phenoxyphenyl)propan-1-ylidene}-1,3-dithiane | HCID 14674059 | 79% |
反応手順
2-Diethoxyphosphoryl-1,3-dithiane, 4.18 g, was dissolved in 40 ml of tetrahydrofuran and 10.5 ml of 1.6 mole hexane solution of n-butyl lithium was dropwise added to the solution in an argon flow at -65° C. The mixture was stirred at the same temperature for an hour. Then, a solution of 36.2 g of 4-phenoxypropiophenone in 15 ml of tetrahydrofuran was dropwise added to the mixture at the same temperature. The reaction mixture was gradually warmed to room temperature overnight. This suspension was poured onto saturated sodium chloride aqueous solution followed by extraction with chloroform. After drying the chloroform phase over magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (chloroform : hexane =1 : 1) to give 4.15 g of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05098928 |
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| 出典データセット | uspto-grants-1992_03 |
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| ORD ID | ord-b15c063df7fe42a486b81c6326eca2d4 |
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| 出典メモ | uspto-grants-1992_03 |
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