関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Chloro-5-nitroanisole | HCID 70519 | — |
| 反応物 | 4-Chlorobenzyl cyanide | HCID 241582 | — |
| 触媒 | Benzyl triethylammonium chloride | HCID 66133 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | alpha-(4-Chlorophenyl)-2-methoxy-4-nitrobenzeneacetonitrile | HCID 23035215 | — |
反応手順
To a stirred mixture of 68 parts of 1-chloro-2-methoxy-4-nitrobenzene, 230 parts of a sodium hydroxide solution 50%, 5 parts of N,N,N-triethylbenzenemethanaminium chloride and 360 parts of tetrahydrofuran is added dropwise, during a 5 minutes period, a solution of 43.2 parts of 4-chlorobenzeneacetonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 4 hours at 60° C. The reaction mixture is poured into 2000 parts of crushed ice. The whole is acidified with concentrated hydrochloric acid. The layers are separated. The aqueous phase is extracted with dichloromethane. The combined extracts are dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding α-(4-chlorophenyl)-2-methoxy-4-nitrobenzeneacetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04767760 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-fff9ae469d1a457387a4a6f72779f1b8 |
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| 出典メモ | uspto-grants-1988_08 |
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