関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4-Dichlorobenzyl chloride | HCID 7212 | — |
| 反応物 | Methyl phenylacetate | HCID 7559 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 2,4-dichloro-alpha-phenylbenzenepropanoate | HCID 21499609 | — |
反応手順
A mixture of 30 parts of methyl benzeneacetate, 6.8 parts of sodium hydride dispersion 78%, 135 parts of N,N-dimethylformamide and 180 parts of benzene is stirred for 1 hour at room temperature, while nitrogen gas is introduced. Another 90 parts of benzene is added. Then there is added dropwise, during a 30 minutes-period, a solution of 43.4 parts of 1,3-dichloro-4-(chloromethyl)benzene in 45 parts of N,N-dimethylformamide. Upon completion, stirring is continued for 30 minutes at room temperature. The reaction mixture is poured onto water and the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is distilled, yielding 26.5 parts of methyl 2,4-dichloro-α-phenylbenzenepropanoate; bp. 140°-145° C at 0.05 mm. pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03991201 |
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| 出典データセット | uspto-grants-1976_11 |
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| ORD ID | ord-ecd323c52d5446afb5cfdd0746570e8f |
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| 出典メモ | uspto-grants-1976_11 |
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