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2,2-Dimethylcyclohexan-1-one → 2-Isopropyl-3-carboethoxy-4-(4-fluorophenyl)-5,6,7,8-tetrahydro-8,8-dimethylquinoline

HRID 324882
Notes
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Reaction equation

HRID 324882 reaction equation
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH3:11][C:12]1([CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14][C:13]1=O.[F:20][C:21]1[CH:26]=[CH:25][C:24]([CH:27]=[C:28]([C:32](=O)[CH:33]([CH3:35])[CH3:34])[C:29]([OH:31])=[O:30])=[CH:23][CH:22]=1.CC(OCC1C2C(=CC=CC=2)C(CO[C:58]([CH3:60])=O)=C2C=1C=CC=C2)=O.C([O-])(=O)C.[NH4+:65]>C1COCC1.C([O-])(=O)C.[Cu+2].C([O-])(=O)C.C(Cl)Cl.CCCCCC.C(OCC)(=O)C.CCCCCC>[CH:33]([C:32]1[C:28]([C:29]([O:31][CH2:58][CH3:60])=[O:30])=[C:27]([C:24]2[CH:25]=[CH:26][C:21]([F:20])=[CH:22][CH:23]=2)[C:14]2[CH2:15][CH2:16][CH2:17][C:12]([CH3:19])([CH3:11])[C:13]=2[N:65]=1)([CH3:35])[CH3:34]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

10

Reactant 5

HCID 1369292,2-Dimethylcyclohexan-1-oneHCID 517165Ammonium AcetateHCID 613145Acetic acid 10-acetoxymethyl-anthracen-9-ylmethyl esterHCID 2733832Lithium hexamethyldisilazaneHCID 544250042-[(4-Fluorophenyl)methylene]-4-methyl-3-oxopentanoic Acid

Product 1

HCID 22005056
2-Isopropyl-3-carboethoxy-4-(4-fluorophenyl)-5,6,7,8-tetrahydro-8,8-dimethylquinoline

Reagents, catalysts & solvents 4

HCID 8895Cupric acetateCatalystHCID 8028TetrahydrofuranSolventHCID 21226206Ethyl acetate hexaneSolventHCID 21226440Methylenechloride HexaneSolvent

Procedure

To a solution of lithium bis(trimethylsilyl)amide (1.0 M/THF, 2 eq. 13.6 mL) in THF (15 mL) was added 2,2-dimethylcyclohexanone (1.88 mL, 13.6 mmol) at −78° C. The reaction was stirred for 15 minutes, and then the intermediate obtained in Step A (3 g, 11.4 mmol) was added dropwise. The reaction was stirred overnight and allowed to warm to room temperature. To the crude product was added acetic add (19.4 mL), ammonium acetate (2.62 g, 34.0 mmol) and copper acetate (5.14 g, 28.3 mmol). The reaction mixture was heated at 100° C. and the THF was removed by distillation. The reaction was heated to 130° C. and allowed to reflux for 24 hours. Ethyl acetate (100 mL) was added and washed with sodium bicarbonate (2×30 mL), water (2×20 mL), brine (2×20 mL), dried with MgSO4, filtered, and concentrated to afford an oil. Flash chromatography (5% ethyl acetate/hexane) afforded a white solid (1.36, 3.7 mmol, 32%). 1H NMR (300 MHz, CDCl3): δ 7.17 (m, 2H), 7.08 (m, 2H), 3.98 (q, J=7.4 Hz, 2H), 3.03 (septet, J=7.0 Hz, 1H), 2.35 (t, J=5.9 Hz, 2H), 1.70 (m, 4H), 1.36 (s, 6H), 1.31 (d, J=4.1 Hz, 6H), 0.965 (t, J=7.4 Hz, 3H). FAB-MS: calculated for (C23H28FNO) 369, found 370 (M+H. mp 124-126° C. Rf=0.6 (50% CH2Cl2/hexane).

Workup

  1. stirringThe reaction was stirred overnight
  2. temperatureThe reaction mixture was heated at 100° C.
  3. customthe THF was removed by distillation
  4. temperatureThe reaction was heated to 130° C.
  5. temperatureto reflux for 24 hours
  6. additionEthyl acetate (100 mL) was added
  7. washwashed with sodium bicarbonate (2×30 mL), water (2×20 mL), brine (2×20 mL)
  8. dry with materialdried with MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customto afford an oil

Sources & evidence

ORD record
ord-a17314e3a38d4910bbbeb42d193a90d5
Source dataset
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06218431B1

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes