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

HRID 1090778ノート

反応式

HRID 1090778 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 10.6g of 2-carbo-propoxy-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 10.6g of 2-carbo-propoxy-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-1dcb488f5d074f87a93e8f90dc8ab740
出典データセット
uspto-grants-1992_01
特許番号
US05082849

反応ノート

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