Vanillin → 3-Methoxy-4-(methoxymethoxy)benzaldehyde

HRID 1030691노트

반응식

HRID 1030691 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:9]=[O:10])[CH:6]=[CH:5][C:4]=1[OH:11].C(=O)([O-])[O-].[K+].[K+].[CH3:18][O:19][CH2:20]Cl>C(C1C=CC=CC=1)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:6]=[CH:5][C:4]=1[O:11][CH2:18][O:19][CH3:20])[CH:9]=[O:10]

참가 물질

5

반응물 3

HCID 1183VanillinHCID 7864Chloromethyl Methyl EtherHCID 11430Potassium Carbonate

생성물 1

HCID 796613-Methoxy-4-(methoxymethoxy)benzaldehyde수율 53.1%

시약·촉매·용매 1

HCID 7410Acetophenone용매

실험 절차

To 14.0 g of vaniline and 51.0 g of potassium carbonate was added 280 ml of acetophenone, and chloromethyl methyl ether was further added and the mixture was refluxed for 1 hour. The reaction liquid was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. The reaction mixture was dissolved in ether, washed with water, shaken with a saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The concentrate was subjected to the column chromatography [230-400 mesh Kieselgel; eluting solvent=hexane/ethyl acetate (2/1)] to obtain 9.6 g (yield=53.1%) of 3-methoxy-4-methoxymethoxybenzaldehyde.

후처리

  1. additionwas further added
  2. temperaturethe mixture was refluxed for 1 hour
  3. customThe reaction liquid
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. dissolutionThe reaction mixture was dissolved in ether
  7. washwashed with water
  8. dry with materialdried with anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-eb2a940fb7c54570abe6147f97a86483
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106871

반응 노트

불러오는 중…