Ethylene Glycol → 2-Pyridinyl-1,3-dioxolane

HRID 742438ノート

反応式

HRID 742438 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]=[O:8].[CH2:9](O)[CH2:10][OH:11].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[O:8]1[CH2:9][CH2:10][O:11][CH:7]1[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 142732-PyridinecarboxaldehydeHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 797732-Pyridinyl-1,3-dioxolane収率 67%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2-pyridinecarboxaldehyde (500 g, 4.67 mol), 561 mL of ethylene glycol, and 234 g of p-toluenesulfonic acid monohydrate in 5.8 L of toluene was heated to reflux while distilling (azeotropic) water formed during the reaction. The solvent was removed in vacuo and the residue was distilled to afford 475 g (67%) of 2-(1,3-dioxolan-2-yl)pyridine (Formula V: R1 =H).

後処理

  1. temperaturewas heated
  2. temperatureto reflux
  3. distillationwhile distilling (azeotropic) water
  4. customformed during the reaction
  5. customThe solvent was removed in vacuo
  6. distillationthe residue was distilled

出典と根拠

ORDレコード
ord-4e760bafeccd4509b7101e1c9747c6d6
出典データセット
uspto-grants-1996_09
特許番号
US05554620

反応ノート

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