Sulfuric Acid → Methyl 4-formylmethyloxybenzoate

HRID 359069ノート

反応式

HRID 359069 の反応式
C([O:3][CH:4](OCC)[CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][CH:8]=1)C.S(=O)(=O)(O)O>O1CCOCC1>[CH:4]([CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][CH:8]=1)=[O:3]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 10084384Methyl 4-(2,2-diethoxyethoxy)benzoate

生成物 1

HCID 11636984Methyl 4-formylmethyloxybenzoate収率 92.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
70 °C

実験手順

Methyl 4-(2,2-diethoxyethoxy)benzoate (36.29 g) was dissolved in dioxane (100 ml), added thereto 2N sulfuric acid (200 ml), and the mixture was heated with stirring at 70° C. for 6 hours. After concentrated under reduced pressure to about half volume, it was diluted with water in two fold, and concentrated again under reduced pressure. The precipitate was collected by filtration, and washed successively with aqueous sodium hydrogencarbonate solution and water to give methyl 4-formylmethoxybenzoate (24.39 g). mp. 58°-60° C.

後処理

  1. additionadded
  2. concentrationAfter concentrated under reduced pressure to about half volume, it
  3. additionwas diluted with water in two fold
  4. concentrationconcentrated again under reduced pressure
  5. filtrationThe precipitate was collected by filtration
  6. washwashed successively with aqueous sodium hydrogencarbonate solution and water

出典と根拠

ORDレコード
ord-0927a61171e64dccacce81c9d49f6f22
出典データセット
uspto-grants-1991_03
特許番号
US04999378

反応ノート

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