Diethyl Ether → HCID 131710314, compound

HRID 1657826Notes

Reaction equation

HRID 1657826 reaction equation
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][N:10]1[CH2:15][CH2:14][CH2:13][CH:12]([CH2:16][C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=2)=[O:18])[CH2:11]1.C(OCC)C>C(OCC)(=O)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][N:10]1[CH2:15][CH2:14][CH2:13][CH:12]([CH2:16][C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=2)=[O:18])[CH2:11]1

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 444266Maleic AcidHCID 21530352HCID 21530352, compound

Product 1

HCID 131710314HCID 131710314, compoundYield 75.6%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To a solution of 2.2 g of maleic acid in 40 ml of ethyl acetate was added 3.9 g of 1-methyl-3-(3-fluorophenacyl)-piperidine, followed by the addition of diethyl ether. The oil which separated was induced to crystallize and the resulting crystals were isolated by filtration and recrystallized from ethyl acetate to give 4.4 g of 1-methyl-3-(3-fluorophenacyl)-piperidine, maleate salt. The following elemental analysis was obtained;

Workup

  1. customThe oil which separated
  2. customto crystallize
  3. customthe resulting crystals were isolated by filtration
  4. customrecrystallized from ethyl acetate

Sources & evidence

ORD record
ord-4b4f017b9d314b589cd75ee88e909c10
Source dataset
uspto-grants-1976_06
Patent number
US03962257

Reaction notes

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