関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Dimethoxybenzoic acid | HCID 7052 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Bromo-2,4-dimethoxybenzoic acid | HCID 13505097 | 96% |
反応手順
2,4-Dimethoxybenzoic acid (30.0 g) was suspended in acetic acid (180 mL). A bromine (27.6 g)/acetic acid (60 mL) solution was slowly added dropwise to the suspension and, after completion of the dropwise addition, the mixture was stirred at 25° C. for 2 hrs, and the termination of the reaction was confirmed by HPLC. An aqueous solution of sodium sulfite (2.10 g) and water (360 mL) was added dropwise to the reaction mixture. After completion of the dropwise addition, the mixture was stirred at 25° C. for 1 hr. Precipitated crystals were filtered, washed 4 times with water (150 mL), and vacuum dried to give 5-bromo-2,4-dimethoxybenzoic acid as white crystals (41.2 g) (96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08383819B2 |
|---|
| 出典データセット | uspto-grants-2013_02 |
|---|
| ORD ID | ord-ea30f8672b05425dab6dc8b277aca716 |
|---|
| 出典メモ | uspto-grants-2013_02 |
|---|