Bromine → 5-Bromo-2-hydroxy-4-methoxybenzaldehyde

HRID 396593

反応式

HRID 396593 の反応式
[OH:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[Br:12]Br>ClCCl.CCOC(C)=O>[Br:12][C:7]1[C:8]([O:10][CH3:11])=[CH:9][C:2]([OH:1])=[C:3]([CH:6]=1)[CH:4]=[O:5]

参加物

5

反応物 2

HCID 24408BromineHCID 696002-Hydroxy-4-Methoxybenzaldehyde

生成物 1

HCID 8181085-Bromo-2-hydroxy-4-methoxybenzaldehyde収率 84.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Ex-62A: A solution of 2-hydroxy-4-methoxybenzaldehyde (3.03 g, 20 mmol) in 25 mL of dichloromethane was cooled to 0° C. and treated dropwise with a solution of bromine (3.41 g, 21 mmol) in 10 mL of dichloromethane. The reaction mixture was stirred at 0° C. for 1.5 hours. The solvent was removed by rotary evaporation to give a residue. The residue was taken up in EtOAc and washed with 3 portions of water. The organic layer was dried over MgSO4. The drying agent was removed by filtration, and solvent was removed by rotary evaporation to give 3.9 g of the desired 5-bromo-2-hydroxy-4-methoxybenzaldehyde as a solid, m.p. 111-115° C.

後処理

  1. customThe solvent was removed by rotary evaporation
  2. customto give a residue
  3. washwashed with 3 portions of water
  4. dry with materialThe organic layer was dried over MgSO4
  5. customThe drying agent was removed by filtration, and solvent
  6. customwas removed by rotary evaporation

出典と根拠

ORDレコード
ord-e385bc02cc6c425bae57c8d05128fab0
出典データセット
uspto-grants-2003_08
特許番号
US06608101B1

関連ノート

読み込み中…