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Pyridine → 4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one

HRID 2084610
Notes
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Reaction equation

HRID 2084610 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[CH2:15]CC(O)=O)=[CH:4][CH:3]=1.[OH-:20].[Na+].S(Cl)(Cl)=O.S(=O)=O.N1C=CC=CC=1.[CH2:35]1[O:39][C:38]2[CH:40]=[C:41]([OH:44])[CH:42]=[CH:43][C:37]=2[O:36]1>C(O)C.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[C:15]([O:44][C:41]2[CH:42]=[CH:43][C:37]3[O:36][CH2:35][O:39][C:38]=3[CH:40]=2)=[O:20])=[CH:6][CH:7]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 6

HCID 1049PyridineHCID 1119Sulfur DioxideHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 68289SesamolHCID 227338414-(4-Fluorophenyl)-3-carboxyethylpiperidin-6-one

Product 1

HCID 22733847
4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one
Yield 51.2%

Reagents, catalysts & solvents 2

HCID 702EthanolSolvent2×HCID 6212ChloroformSolvent

Conditions

Temperature
60 °C

Procedure

A solution of 4-(4-fluorophenyl)-3-carboxyethylpiperidin-6-one (0.5 g, 1.88 mmol, trans/cis ratio 56:44) in ethanol (10 ml) was added to a solution of sodium hydroxide (0.08 g, 2 mmol) in 95% ethanol (5 ml) and the mixture heated for 4 hours at 60° C. The solvent was removed at reduced pressure and the residue of water removed by distillation with toluene. The residue was suspended in dichloromethane (5 ml), treated with a solution of thionyl chloride (0.24 g, 2 mmol), and the mixture was brought to reflux. After 1 hour evolution of sulphur dioxide ceased, so the mixture was cooled to room temperature and treated with pyridine (0.16 g, 2 mmol) followed by a solution of sesamol (0.24 g, 1.75 mmol) in chloroform (2.5 ml). The resulting mixture was brought to reflux, heated for 4 hours, and stirred at ambient temperature for 2 days. The solvent was then removed at reduced pressure and the residue treated with water (5 ml), then extracted with ethyl acetate (20 and 10 ml). The organic extracts were combined, washed with brine (20 ml), dried over anhydrous sodium sulphate, filtered and evaporated to give the title compound (0.32 g).

Workup

  1. customThe solvent was removed at reduced pressure
  2. customthe residue of water removed by distillation with toluene
  3. temperatureto reflux
  4. temperaturewas cooled to room temperature
  5. temperatureto reflux
  6. temperatureheated for 4 hours
  7. customThe solvent was then removed at reduced pressure
  8. additionthe residue treated with water (5 ml)
  9. extractionextracted with ethyl acetate (20 and 10 ml)
  10. washwashed with brine (20 ml)
  11. dry with materialdried over anhydrous sodium sulphate
  12. filtrationfiltered
  13. customevaporated

Sources & evidence

ORD record
ord-ca0b17549cdc40728873bf781931c97d
Source dataset
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06716985B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes