関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1-(Triphenylphosphoranylidene)acetone | HCID 15038 | — |
| 反応物 | 2'-(2,4-Difluorophenoxy)-4'-formylmethanesulfonanilide | HCID 10404154 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2'-(2,4-Difluorophenoxy)-4'-(3-oxo-1-butenyl)methanesulfonanilide | HCID 53916136 | 38.7% |
反応手順
A mixture of 2'-(2,4-difluorophenoxy)-4'-formylmethanesulfonanilide (2.3 g) and triphenylphosphoranylideneacetone (2.3 g) in dimethylsulfoxide (10 ml) was stirred for 13 hours at 80° C. After cooling of the mixture, ethyl acetate was added, and the resulting mixture was washed with water, then dried. The ethyl acetate layer was evaporated to dryness and the residue was purified by column chromatography on silica gel (80 g) eluting with a mixture of chloroform and methanol (200:1) and further recrystallized from ethanol to give pale yellow needles of 2'-(2,4-difluorophenoxy)-4'-(3-oxo-1-butenyl)methanesulfonanilide (1.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04866091 |
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| 出典データセット | uspto-grants-1989_09 |
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| ORD ID | ord-87f4f2976bdf4a429ea6a3e28c5d5549 |
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| 出典メモ | uspto-grants-1989_09 |
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