Methanol → HCID 19793837, compound
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
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
- customThe excess methanol is evaporated off in a rotary evaporator
- washwashed with water
- dry with materialThe organic phase is dried over sodium sulfate
- concentrationconcentrated to dryness by evaporation
- 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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