Water → 5-Bromo-2,4-dimethoxybenzoic acid

HRID 391233

反応式

HRID 391233 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].[Br:14]Br.S([O-])([O-])=O.[Na+].[Na+].O>C(O)(=O)C>[Br:14][C:9]1[C:10]([O:12][CH3:13])=[CH:11][C:3]([O:2][CH3:1])=[C:4]([CH:8]=1)[C:5]([OH:7])=[O:6]

参加物

6

反応物 4

HCID 962WaterHCID 70522,4-Dimethoxybenzoic acidHCID 24408BromineHCID 24437Sodium Sulfite

生成物 1

HCID 135050975-Bromo-2,4-dimethoxybenzoic acid収率 96%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
25 °C

実験手順

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%).

後処理

  1. additionafter completion of the dropwise addition
  2. additionAfter completion of the dropwise addition
  3. stirringthe mixture was stirred at 25° C. for 1 hr
  4. customPrecipitated crystals
  5. filtrationwere filtered
  6. washwashed 4 times with water (150 mL), and vacuum
  7. customdried

出典と根拠

ORDレコード
ord-ea30f8672b05425dab6dc8b277aca716
出典データセット
uspto-grants-2013_02
特許番号
US08383819B2

関連ノート

読み込み中…