Acrolein → 6-Hydroxychromene-3-carboxaldehyde

HRID 394695

반응식

HRID 394695 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][C:3]=1[CH:4]=O.[CH:11]([CH:13]=[CH2:14])=[O:12].C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.O>[OH:10][C:7]1[CH:6]=[C:3]2[C:2](=[CH:9][CH:8]=1)[O:1][CH2:14][C:13]([CH:11]=[O:12])=[CH:4]2

참가 물질

6

반응물 3

HCID 7847AcroleinHCID 11430Potassium CarbonateHCID 709492,5-Dihydroxybenzaldehyde

생성물 1

HCID 47708156-Hydroxychromene-3-carboxaldehyde

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

3 g (21.7 mmol) of 2,5-dihydroxybenzaldehyde and also 2.2 ml (32.6 mmol) of acrolein are added to a suspension of 6 g (43.5 mmol) of potassium carbonate in 50 ml of 1,4-dioxane; the medium is then heated at reflux for 12 hours. The salts are filtered off over Celite; the solvent is then evaporated in vacuo. The residue obtained is taken up in water; the aqueous phase is then extracted with ether. After drying over magnesium sulphate and evaporation of the solvent in vacuo, the crude product is triturated in dichloromethane to yield the title compound in the form of a yellow solid.

후처리

  1. temperaturethe medium is then heated
  2. temperatureat reflux for 12 hours
  3. filtrationThe salts are filtered off over Celite
  4. customthe solvent is then evaporated in vacuo
  5. customThe residue obtained
  6. extractionthe aqueous phase is then extracted with ether
  7. dry with materialAfter drying over magnesium sulphate and evaporation of the solvent in vacuo
  8. customthe crude product is triturated in dichloromethane

출처 및 근거

ORD 기록
ord-f05f9fe6aaf84aceb3adbcadbb4182a8
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602903B2

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