Methanol → HCID 19793837, compound

HRID 1077704Notes

Reaction equation

HRID 1077704 reaction equation
[F:1][C:2]([F:10])=[CH:3][CH2:4][CH2:5][CH2:6][C:7](Cl)=[O:8].N1C=CC=CC=1.[CH3:17][OH:18]>>[CH3:17][O:18][C:7](=[O:8])[CH2:6][CH2:5][CH2:4][CH:3]=[C:2]([F:10])[F:1]

Participants

4

Reactant 3

HCID 887MethanolHCID 1049PyridineHCID 197938396,6-Difluorohex-5-enoic acid chloride

Product 1

HCID 19793837HCID 19793837, compound

Procedure

42.1 g of 6,6-difluorohex-5-enoic acid chloride are added slowly at 10° to 17.6 g of pyridine in 200 ml of methanol. The mixture is then stirred at room temperature for 5 hours. The excess methanol is evaporated off in a rotary evaporator and the residue is taken up in tert-butyl methyl ether and washed with water. The organic phase is dried over sodium sulfate and concentrated to dryness by evaporation. The residue is distilled at 60 mbar. The title compound is obtained in the form of a colourless oil.

Workup

  1. customThe excess methanol is evaporated off in a rotary evaporator
  2. washwashed with water
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. concentrationconcentrated to dryness by evaporation
  5. distillationThe residue is distilled at 60 mbar

Sources & evidence

ORD record
ord-a2b9ebbb225743bca369ecd2e1984fc1
Source dataset
uspto-grants-1996_08
Patent number
US05545630

Reaction notes

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