関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | 4-(4-Fluorophenoxy)-1-methyl-2-nitrobenzene | HCID 3537673 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | E-1-(1-pyrrolidinyl)-2-[2-nitro-4-(4-fluorophenoxy)phenyl]ethylene | HCID 19038053 | 103.4% |
反応手順
2-Nitro-4-(4-fluorophenoxy)toluene (11.8 g, 47.7 mmol), was dissolved in dimethylformamide (90.0 mL) under N2 atmosphere. Dimethylformamide dimethyl acetal (20.2 mL, 143 mmol), and pyrrolidine (4.0 mL, 47.4 mmol) were added via syringe and the reaction mixture was heated at 110° C. for 3 hours. The reaction mixture was cooled to ambient temperature and partitioned between H2O and ether. The organic phase was washed with H2O. The combined aqueous extracts were washed with ether. The ether extracts were combined and dried over Na2SO4, filtered, and concentrated in vacuo to give a viscous oil (16.1 g) which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05643922 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-91ad2b0cc9b648a99f036c8dce7d451b |
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| 出典メモ | uspto-grants-1997_07 |
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