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Potassium Carbonate → 4-(4-Acetyl-3-chlorophenoxy)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Cyanophenol | HCID 13019 | — |
| 反応物 | 2'-Chloro-4'-fluoroacetophenone | HCID 2736507 | — |
| 反応物 | Ethylacetate heptane | HCID 21899848 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 4-(4-Acetyl-3-chlorophenoxy)benzonitrile | HCID 64335501 | — |
反応手順
To a solution 4-cyanophenol (CAS Reg. No. 767-00-0, 1.2 g), 2-chloro-4-fluoroacetophenone (CAS Reg. No. 700-35-6, 1.7 g) in DMA (10 ml) was added K2CO3 (1.66 g). The mixture is refluxed for 5 h. TLC (heptane/EtOAc 2:1) showed complete conversion. Water was added and the mixture was extracted with DCM. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:2) to give the title compound (1.8 g) as yellow oil. MS (m/e)=272.2 [M+H+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138189B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-dc8398acd11a40ffbe7b23aa940ad840 |
| 出典メモ | uspto-grants-2012_03 |