Sulfuric Acid → Methyl 4-formylmethyloxybenzoate

HRID 359069노트

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HRID 359069 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 11636984Methyl 4-formylmethyloxybenzoate수율 92.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0927a61171e64dccacce81c9d49f6f22
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999378

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