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1-Methyl-4-piperidone → 4-[2-(1-Hydroxy-1-methylethyl)phenyl]-1-methylpiperidin-4-ol

HRID 1179278
Notes
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Reaction equation

HRID 1179278 reaction equation
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([OH:11])([CH3:10])[CH3:9].C([Li])CCC.[CH3:17][N:18]1[CH2:23][CH2:22][C:21](=[O:24])[CH2:20][CH2:19]1>O1CCCC1>[OH:11][C:8]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[C:21]1([OH:24])[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]1)([CH3:10])[CH3:9]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 740491-Methyl-4-piperidoneHCID 3295272-(2-Bromophenyl)propan-2-olHCID 178418339Butyllithium

Product 1

HCID 122896704-[2-(1-Hydroxy-1-methylethyl)phenyl]-1-methylpiperidin-4-olYield 58%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Procedure

To a stirred solution of 2-(2-bromophenyl)propan-2-ol (step 1, 6.91 g, 32.1 mmol) in tetrahydrofuran (32 mL) was added dropwise a 1.59 M solution of butyllithium in tetrahydrofuran (46.5 mL, 73.9 mmol) at −78° C. for 20 min and the mixture was stirred for 1 h at the same temperature. To the mixture was added dropwise a solution of 1-methylpiperidin-4-one (5.09 g, 45.0 mmol) in tetrahydrofuran (18 mL) at −78° C. for 10 min. This resulting mixture was slowly warmed up to room temperature and stirred for 18 h at the same temperature. The reaction mixture was quenched by the addition of water, and concentrated to give an orange residue. The crude material was partitioned between diethyl ether and water, and then the organic layer was washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by column chromatography on silica gel (150 g) eluting with hexane/ethyl acetate (5/1), dichloromethane/methanol (10/1), then dichloromethane/methanol/triethylamine (10/1/1) to afford 4.62 g (58%) of the title compound as a slight yellow syrup:

Workup

  1. stirringstirred for 18 h at the same temperature
  2. customThe reaction mixture was quenched by the addition of water
  3. concentrationconcentrated
  4. customto give an orange residue
  5. customThe crude material was partitioned between diethyl ether and water
  6. washthe organic layer was washed with brine
  7. dry with materialdried over sodium sulfate
  8. customevaporated
  9. customThe residue was purified by column chromatography on silica gel (150 g)
  10. washeluting with hexane/ethyl acetate (5/1), dichloromethane/methanol (10/1)

Sources & evidence

ORD record
ord-3492e4628db2461c9d3543f79584ad54
Source dataset
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07279486B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes