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

HRID 1679010

反応式

HRID 1679010 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 2035672-(Phenylmethoxy)-1,3-propanediol収率 87.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4257fb10ad2d44c2af8251846a929550
出典データセット
uspto-grants-1978_03
特許番号
US04077982

関連ノート

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