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Ethylene Glycol → 3-(Pyridin-4-yloxy)propan-1-OL

HRID 1737585
Notes
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Reaction equation

HRID 1737585 reaction equation
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.[CH2:8]([OH:11])[CH2:9]O.[OH-:12].[Na+].[CH3:14]S(C)=O>>[OH:12][CH2:14][CH2:9][CH2:8][O:11][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

HCID 174Ethylene GlycolHCID 679Dimethyl SulfoxideHCID 122884-ChloropyridineHCID 14798Sodium Hydroxide

Product 1

HCID 219360073-(Pyridin-4-yloxy)propan-1-OLYield 45%

Conditions

Temperature
100 °C

Procedure

A mixture of 4-chloropyridine (7 g, 47 mmol), ethylene glycol (17.9 g, 235 mmol) and sodium hydroxide (4.67 g, 195 mmol) in DMSO (80 ml) was heated at 100° C. for 24 hours. Most of the solvent was removed by evaporation and the residue was diluted with ice water. The aqueous mixture was extracted with ethyl acetate, the extracts combined, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with methylene chloride/methanol mixtures (100/0 increasing to 97/3) to give 4-(3-hydroxypropoxy)pyridine (3.2 g, 45%).

Workup

  1. customMost of the solvent was removed by evaporation
  2. additionthe residue was diluted with ice water
  3. extractionThe aqueous mixture was extracted with ethyl acetate
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed by evaporation
  6. customThe residue was purified by column chromatography
  7. washeluting with methylene chloride/methanol mixtures (100/0 increasing to 97/3)

Sources & evidence

ORD record
ord-f61e2bab27ce48c1969a1fd50296fb40
Source dataset
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05962458

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes