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Hydrochloric Acid → Methyl 3-(cyanoacetyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Dimethyl isophthalate | HCID 15088 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 3-(cyanoacetyl)benzoate | HCID 18945177 | — |
反応手順
Potassium tert-butoxide (6.4 g) was added to a solution of dimethyl isophthalate (10.0 g) in acetonitrile (90 ml) at ambient temperature and the mixture was stirred for 1 hour at 60°-64° C. The reaction mixture was added to a solution of conc. hydrochloric acid (4.7 ml) in water (150 ml) and extracted with ethyl acetate. The extract layer was washed with water and dried over magnesium sulfate. Evaporation of the solvent gave a residue, which was purified by column chromatography on silica gel eluting with chloroform. The eluted fractions containing the desired product were collected and evaporated in vacuo to give methyl 3-(cyanoacetyl)benzoate (4.72 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05824691 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-f772dbd880c24b43a232bf96abd46a4f |
| 出典メモ | uspto-grants-1998_10 |