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

HRID 1110899ノート

反応式

HRID 1110899 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e0d75e8be2574821b8ab3955bc35e48b
出典データセット
uspto-grants-1990_12
特許番号
US04977162

反応ノート

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