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

HRID 420863

반응식

HRID 420863 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 109869082-Hydroxy-4,5-dimethoxybenzaldehyde수율 89.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a458774184084d3eb5ffc3084e448d1d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097720B2

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