関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic acid, 2-phenoxy-, ethyl ester | HCID 17365 | — |
| 反応物 | Methyl phenyl sulfone | HCID 18369 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Phenylsulfonyl-2-oxo-3-phenoxypropane | HCID 15080405 | — |
反応手順
n-Butyllithium (8.5 ml, 1.6M in hexane) was added at -72° C. to a solution of methylphenyl sulfone (2.14 g, 13.7 mmol) in 80 ml of tetrahydrofuran. The reaction mixture was then allowed to warm slowly to -20° C. and maintained at this temperature for 25 minutes. It was then recooled to -72° C. and ethyl phenoxyacetate (1.48 g, 8.22 mmol) was added dropwise. The cooling bath was removed, the mixture was stirred at 20° C. for 14 hrs. and then poured into 100 ml of saturated NH4Cl and extracted with diethyl ether. The combined organic extracts were washed with brine, dried over anhydrous magnesium sulfate and the solvent removed under reduced pressure. The crude residue was purified by column chromatography (silica gel, methylene chloride) giving 1-phenylsulfonyl-2-oxo-3-phenoxypropane, the compound of formula (2a), 800 mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04888358 |
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| 出典データセット | uspto-grants-1989_12 |
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| ORD ID | ord-2cd40da7323a4651b90ebe714304744b |
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| 出典メモ | uspto-grants-1989_12 |
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