3,4-dihydro-2H-pyran → HCID 19086554, compound

HRID 1464830Notes

Reaction equation

HRID 1464830 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[OH:9].[O:10]1[CH:15]=[CH:14][CH2:13][CH2:12][CH2:11]1.[OH-].[Na+]>>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[O:9][CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][O:10]1

Participants

4

Reactant 3

HCID 80803,4-dihydro-2H-pyranHCID 14798Sodium HydroxideHCID 1230512,4-Difluorophenol

Product 1

HCID 19086554HCID 19086554, compound

Conditions

Temperature
0 °C

Procedure

260.2 g (2.0 mol) of 2,4-difluorophenol and 252.4 g (3.0 mol) of 3,4-dihydro-2H-pyran are introduced into a 750 ml sulfation flask and cooled to 0° C. One drop of polyphosphoric acid is carefully added to the solution, and the mixture is stirred for a further 16 hours at 0° to 5° C. (check using GC and TLC). The mixture is then reduced alkaline using a little powdered sodium hydroxide. The product is distilled at 119°-120° C. in vacuo (22 mbar). 377 g (88% of theory) of a clear, colourless liquid are obtained.

Workup

  1. distillationThe product is distilled at 119°-120° C. in vacuo (22 mbar)
  2. custom377 g (88% of theory) of a clear, colourless liquid are obtained

Sources & evidence

ORD record
ord-a6ba4ddfb6c343049f8aacad7d1cfcb9
Source dataset
uspto-grants-1994_04
Patent number
US05306600

Reaction notes

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