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Hydrochloric Acid → Methyl (4-cyanophenyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Mesitylene | HCID 7947 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(Bromomethyl)benzonitrile | HCID 86996 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | Pentacarbonyliron(0) | HCID 518773 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl (4-cyanophenyl)acetate | HCID 1512619 | — |
反応手順
30.0 g (0.15 mol) of 4-bromomethyl-benzonitrile, 2.0 ml (0.12 mol) of iron pentacarbonyl, 29.0 g potassium carbonate, 10.0 ml mesitylene and 250 ml absolute methanol are placed in a pressure vessel and about 3.5 l carbon monoxide gas is introduced. The reaction mixture is shaken for 16 hours at ambient temperature, mixed with water, neutralised with hydrochloric acid and extracted with ethyl acetate. The combined organic extracts are washed with sodium hydrogen carbonate solution, dried and evaporated down. The residue is chromatographed on silica gel and eluted with petroleum ether/ethyl acetate (9:1, 8:2 and 7:3). The desired fractions are combined and evaporated down.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06200976B1 |
| 出典データセット | uspto-grants-2001_03 |
| ORD ID | ord-302c30427a344b1c9cdb645005d46293 |
| 出典メモ | uspto-grants-2001_03 |