関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | (4-Chlorophenyl)acetic acid | HCID 15880 | — |
| 反応物 | Methyl 2,4-dichlorobenzoate | HCID 37055 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethan-1-one | HCID 21984867 | 62.2% |
反応手順
420 ml of a 2M solution of the sodium salt of hexamethyldisilazane in THF are cooled to −60° C. under a nitrogen atmosphere, 350 ml of THF are added, then, dropwise, a solution of 57.6 g of 4-chlorophenylacetic acid in 70 ml of THF is added and the mixture is left stirring at −60° C. for one hour. 66 g of methyl 2,4-dichlorobenzoate are subsequently added dropwise at −60° C., the mixture is left stirring at −60° C. for 40 minutes and then the temperature is allowed to rise to 0° C. The reaction mixture is poured onto an ice/1 liter of 2N HCl mixture and extracted with ether, the organic phase is dried over Na2SO4, the solvent is concentrated under vacuum to a volume of 150 ml, 200 ml of pentane are added and the crystalline product formed is filtered off. 60 g of the expected compound are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07589120B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-64d675e194034178825574bb6bd7d65c |
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| 出典メモ | uspto-grants-2009_09 |
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