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Hydrochloric Acid → 1-Benzyl-4-(4-phenylbutylidene)piperidine

HRID 1068133
Notes
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Reaction equation

HRID 1068133 reaction equation
C[Si]([N-][Si](C)(C)C)(C)C.[K+].C1COCC1.[Br-].[C:17]1([CH2:23][CH2:24][CH2:25][CH2:26][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[CH2:46]([N:53]1[CH2:58][CH2:57][C:56](=O)[CH2:55][CH2:54]1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1.Cl>C1(C)C=CC=CC=1>[CH2:46]([N:53]1[CH2:58][CH2:57][C:56](=[CH:26][CH2:25][CH2:24][CH2:23][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:55][CH2:54]1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 192201-Benzyl-4-piperidoneHCID 3251421Potassium bis(trimethylsilyl)amideHCID 18187515(4-Phenylbutyl)triphenylphosphonium bromide

Product 1

HCID 181876891-Benzyl-4-(4-phenylbutylidene)piperidine

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent3×

Procedure

A 0.62M solution of potassium bis(trimethylsilyl)amide in THF (180 mL, 112 mmol) in toluene (250 mL) was added to a mixture of (4-phenylbut-1-yl)triphenylphosphonium bromide (from the Step B) (53 g) in toluene (250 mL) in an ice bath over 15 min with stirring under nitrogen. After stirring for a further 15 min, a solution of 1-benzyl-4-piperidone (16.9 g) in toluene (100 mL) was added over 30 min with stirring. The reaction mixture was allowed to warm to rt over 15 h. The reaction mixture was then poured into cold 1N HCl (400 mL) and the layers were separated. The organic layer was extracted with two more portions of 1N HCl. The combined cloudy HCl solution and an oil layer in between were washed with toluene (200 mL) before the aqueous layer was basified by the addition of potassium hyroxide (30 g). The aqueous layer was extracted with ether (3×150 mL) and the combined organic layers were washed with water and brine, dried over sodium sulfate and concentrated. The crude product was purified by FC (10˜15% ethyl acetate in hexanes having 4% (v/v) TEA) to give the title compound (16 g) as a colorless oil. Rf: 0.47 (20% ethyl acetate in hexanes having 4% (v/v) TEA). 1H NMR (500 MHz, CDCl3): δ7.26-7.38 (m, 7 H), 7.18-7.21 (m, 3 H), 5.18 (t, J=7.4 Hz, 1 H), 3.54 (s, 2 H), 2.61-2.64 (m, 2 H), 2.42-2.49 (m, 4 H), 2.22-2.27 (m, 4 H), 2.02-2.07 (m, 2 H), 1.65-1.71 (m, 2 H).

Workup

  1. stirringAfter stirring for a further 15 min
  2. stirringwith stirring
  3. customthe layers were separated
  4. extractionThe organic layer was extracted with two more portions of 1N HCl
  5. washThe combined cloudy HCl solution and an oil layer in between were washed with toluene (200 mL) before the aqueous layer
  6. additionwas basified by the addition of potassium hyroxide (30 g)
  7. extractionThe aqueous layer was extracted with ether (3×150 mL)
  8. washthe combined organic layers were washed with water and brine
  9. dry with materialdried over sodium sulfate
  10. concentrationconcentrated
  11. customThe crude product was purified by FC (10˜15% ethyl acetate in hexanes having 4% (v/v) TEA)

Sources & evidence

ORD record
ord-93fcd40e03384b329a1e2e41b33176de
Source dataset
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06248755B1

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes