Water → 2-(Phenylmethoxy)-1,3-propanediol

HRID 1679010

반응식

HRID 1679010 반응식
[CH2:1]([O:8][CH:9]1[CH2:14][O:13]C(C2C=CC=CC=2)[O:11][CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(=O)(=O)(O)O.O>C(O)C>[CH2:1]([O:8][CH:9]([CH2:10][OH:11])[CH2:14][OH:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 2630835-(Benzyloxy)-2-phenyl-1,3-dioxane

생성물 1

HCID 2035672-(Phenylmethoxy)-1,3-propanediol수율 87.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 370 g of 5-benzyloxy-2-phenyl-1,3-dioxane and 35 ml of concentrated sulfuric acid in a medium of 750 ml of water and 1.2 l of ethanol was refluxed for 2 hours. The ethanol was then removed by evaporation under reduced pressure, and by-product benzaldehyde was removed by steam distillation. The aqueous mixture was saturated with potassium carbonate, and the product was extracted from the aqueous medium with ether. The ethereal solution was dried (MgSO4) and evaporated under reduced pressure to give solid product, which upon recrystallization from a benzene/ligroine system gave 218 g of 2-benzyloxy-1,3-propanediol, m.p. 38°-39° C.

후처리

  1. customThe ethanol was then removed by evaporation under reduced pressure, and by-product benzaldehyde
  2. customwas removed by steam distillation
  3. extractionthe product was extracted from the aqueous medium with ether
  4. dry with materialThe ethereal solution was dried (MgSO4)
  5. customevaporated under reduced pressure
  6. customto give solid product, which
  7. customupon recrystallization from a benzene/ligroine system

출처 및 근거

ORD 기록
ord-4257fb10ad2d44c2af8251846a929550
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04077982

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