化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → tert-Butyl 6-bromopicolinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Bromo-picolinic acid | HCID 21081564 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | tert-Butyl 6-bromopicolinate | HCID 23432991 | 79% |
反応手順
p-Toluenesulfonyl chloride (9.0 g, 47.2 mmol) was added portionwise to a mixture of 2-bromo-picolinic acid (4.02 g, 19.9 mmol) in tert-butanol (36 mL) and pyridine (10.8 mL, 134 mmol) at 0° C. and the mixture was stirred at rt for 14 hours. An aqueous solution of sodium bicarbonate was slowly added. The precipitate was filtered, washed with water and dried in vacuo to provide 4.04 g (79%) of the desired product tert-butyl 6-bromopicolinate (25A): 1H NMR (300 MHz, CDCl3) δ 7.97 (1H, dd), 7.64 (2H, m), 1.62 (9H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08518970B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-05ebd5e184f24c2981849bc5b14d4f4c |
| 出典メモ | uspto-grants-2013_08 |