1-Propanol → 2-carbopropoxy-6-hydroxy-4-oxo-4H-1-benzopyran

HRID 1110899노트

반응식

HRID 1110899 반응식
[C:1]([C:4]1[O:5][C:6]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][C:7]=2[C:8](=[O:10])[CH:9]=1)([OH:3])=[O:2].[CH2:16](O)[CH2:17][CH3:18]>S(=O)(=O)(O)O>[C:1]([C:4]1[O:5][C:6]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][C:7]=2[C:8](=[O:10])[CH:9]=1)([O:3][CH2:16][CH2:17][CH3:18])=[O:2]

참가 물질

4

반응물 2

HCID 10311-PropanolHCID 152253396-Hydroxy-4H-4-oxochromene-2-carboxylic acid

생성물 1

HCID 199138472-carbopropoxy-6-hydroxy-4-oxo-4H-1-benzopyran

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

14.14 g (49.2 mmoles) of 2-carboxy-6-hydroxy-4-oxo-4H-1-benzopyran is dissolved in 200 ml of n-propanol and 1 drop of concentrated sulfuric acid is added. The mixture is refluxed for 30 hours, concentrated. The resulting solid is suspended in water, neutralized with sodium bicarbonate and filtered, washing the solid with water, then drying. This gives 10.6 g of 2-carbopropoxy-6-hydroxy-4-oxo-4H-1-benzopyran as a solid which is purified by recrystallization from n-propanol/acetone or by HPLC.

후처리

  1. temperatureThe mixture is refluxed for 30 hours
  2. concentrationconcentrated
  3. filtrationfiltered
  4. washwashing the solid with water
  5. customdrying
  6. customThis gives 10.6 g of 2-carbopropoxy-6-hydroxy-4-oxo-4H-1-benzopyran as a solid which is purified by recrystallization from n-propanol/acetone or by HPLC

출처 및 근거

ORD 기록
ord-e0d75e8be2574821b8ab3955bc35e48b
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04977162

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