関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1,3-Benzenedicarboxylic acid, 4-methyl-, 1,3-dimethyl ester | HCID 89971 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Dimethyl 4-(bromomethyl)isophthalate | HCID 14920817 | 72.6% |
反応手順
To a solution of dimethyl 4-methylisophthlate (Chemical Formula 4) (4 g, 19.2 mmol) in distilled dichloromethane were added N-bromosuccinimide (NBS, 4.8 g, 26.9 mmol) and benzoic peroxyanhydride (0.47 g, 19.2 mmol), followed by reaction at 80° C. for 24 hours in a pressure vessel with constant stirring. The reaction progress was monitored by TLC [Hex:EA=3:1]. When the reaction was detected to have reached completion, saturated NaHCO3 was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer thus formed was dried over anhydrous MgSO4, filtered and concentrated in a vacuum. The purification of the concentrate through column chromatography [Hexane: EtOAc=20:1] produced 4 g of dimethyl 4-(bromomethyl)isophthalate (Chemical Formula 5) (70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08148402B2 |
|---|
| 出典データセット | uspto-grants-2012_04 |
|---|
| ORD ID | ord-3aeca7e6f54f45658f5315fd3ee41353 |
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| 出典メモ | uspto-grants-2012_04 |
|---|
