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Pyridine → 2-Pivaloyloxy-5-bromo-6-methylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | 3-Bromo-6-hydroxy-2-methylbenzoic acid | HCID 11053451 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Pivaloyloxy-5-bromo-6-methylbenzoic acid | HCID 23293234 | — |
反応手順
A mixture of 1B (6.45 g, 28 mmol), pivaloylchloride (3.62 g, 30 mmol), tetrahydrofuran (60 ml) and pyridine (2.45 ml) is stirred at room temperature for 16 hours. The reaction mixture is diluted with water and ethyl acetate. The organic phase is washed with water twice. The organic phase is concentrated in vacuo and the residue is re-crystallized from petrol ethers/diisopropylether (9:1 v/v) yielding the pure product as a white crystals, 6.3 g, (71.6%), mp. 144-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06127570 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-32e49ff7cf8e465b838d4cd342ec1d7d |
| 出典メモ | uspto-grants-2000_10 |