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4-Hydroxybenzaldehyde → 2-Chloro-4-(4-formylphenoxy)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-4-fluorobenzonitrile | HCID 109000 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-4-(4-formylphenoxy)benzonitrile | HCID 59730014 | — |
反応手順
4-Hydroxy benzaldehyde (1 equiv), 2-chloro-4-fluorobenzonitrile (1 equiv) and K2CO3 (2.5 equiv) in anhydrous DMF (0.2 M) were heated at 110° C. under nitrogen during 1 hour (the reaction can be monitored by tlc). After cooling down to room temperature, the reaction mixture was poured into water and extracted with ethyl acetate (3×50 mL). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum (toluene was added to aid DMF evaporation). The crude mixture was purified by flash chromatography using hexanes/ethyl acetate (4:1) as eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381719B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-d284882dfca44239b0836b3ccd0b53d2 |
| 出典メモ | uspto-grants-2008_06 |