Hydrochloric Acid → 2-Hydroxy-4,5-dimethoxybenzaldehyde

HRID 420863ノート

反応式

HRID 420863 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:12]([O:17]C)=[CH:13][C:14]=1[O:15][CH3:16])[CH:10]=[O:11].O.Cl>ClCCl>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:12]([OH:17])=[CH:13][C:14]=1[O:15][CH3:16])[CH:10]=[O:11]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 205252,4,5-TrimethoxybenzaldehydeHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 109869082-Hydroxy-4,5-dimethoxybenzaldehyde収率 89.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

In a three-necked flask, disperse 40.8 g of aluminium chloride in 200 ml of dichloromethane with stirring. Cool the solution to 0° C. Pour in dropwise a solution of 20 g (0.101 mol) of 3,4,6-trimethoxybenzaldehyde dissolved in 100 ml of dichloromethane. Allow the temperature to rise again to 19° C. and stir for 45 min. Hydrolyse the reaction mixture with 400 g of water and ice and then add 100 ml of 1N HCl and stir for 30 minutes. Allow to separate and then extract with 200 ml of dichloromethane. The organic phase is washed with 100 ml of 1N HCl, 100 ml of water and 100 ml of saturated aqueous NaCl solution, and then dried over MgSO4, filtered and evaporated to dryness. 16.4 g of title product are obtained.

後処理

  1. customto rise again to 19° C.
  2. stirringstir for 45 min
  3. stirringstir for 30 minutes
  4. customAllow to separate
  5. extractionextract with 200 ml of dichloromethane
  6. washThe organic phase is washed with 100 ml of 1N HCl, 100 ml of water and 100 ml of saturated aqueous NaCl solution
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-a458774184084d3eb5ffc3084e448d1d
出典データセット
uspto-grants-2012_01
特許番号
US08097720B2

反応ノート

読み込み中…