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Water → (S)-6-chloro-2-(alpha-methylbenzyl) 3,4-dihydronaphthalene

HRID 2255273
Notes
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Reaction equation

HRID 2255273 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH2:8][C:7](=O)[CH2:6][CH2:5]2.[CH3:13][C@H:14]([NH2:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[OH2:22].[C:23]1([CH3:29])C=CC=C[CH:24]=1>>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]2[C:8]3[CH2:29][CH2:23][C:24](=[O:22])[N:21]([C@@H:14]([CH3:13])[C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[C:7]=3[CH2:6][CH2:5][C:4]=2[CH:3]=1.[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C@H:14]([CH3:13])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:6][CH2:5]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 1140TolueneHCID 758181-Phenethylamine, (-)-HCID 44561396-Chloro-2-tetralone

Product 2

HCID 53932928(S)-6-chloro-2-(alpha-methylbenzyl) 3,4-dihydronaphthaleneHCID 54339907(S)-(-)-8-chloro-4-(alpha-methylbenzyl)-1,2,3,4,5,6-hexahydrobenzo[f]quinolin-3-one

Procedure

To a stirred solution of 6-chloro-2-tetralone (1.0 equiv., 100.0 mmol., 18.06 g) in toluene (300 ml) was added (S)-(-)-α-methylbenzylamine (1.0 equiv., 100.0 mmol., 12.9 ml). The mixture was heated at reflux for 3 hrs with the azeotropic removal of water (Dean Stark). The cooled reaction mixture was concentrated in vacuo to give the enamine, (S)-6-chloro-2-(α-methylbenzyl) 3,4-dihydronaphthalene, as a purple oil. The oil was taken up in chloroform (150 ml) and saturated aqueous sodium bicarbonate was added (150 ml). The vigorously stirred mixture was treated with acryloyl chloride (1.05 equiv., 105.0 mmol., 8.5 ml) dropwise over 5 min. The reaction mixture was allowed to stir at ambient temperature for 20 min., then diluted with chloroform and the layers separated. The aqueous layer was extracted with chloroform (1×). The combined organics were washed with brine (1×), dried (Na2SO4), and concentrated in vacuo to give 37.9 g of a black oil. The crude oil was subjected to HPLC on silica gel (gradient elution with hexanes increasing to 25% ethyl acetate/hexanes) to give 19.03 g of a purple oil which was further purified by flash chromatography on silica gel (elution with 20% ethyl acetate/hexanes) to give 17.96 g, 53% yield of the title compound as a brown glass which was homogeneous by HPLC analysis (reverse phase, C18, mobile phase: 60% acetonitrile/0.5% aqueous ammonium acetate buffer), thin layer chromatography (Silica gel, Rf =-0.5, developed with 40% ethyl acetate/hexanes), and 300MHz 1H NMR analysis. FDMS: m/e=337. α[D]589 =-24.75 (c=1.0, CHCl3).

Workup

  1. temperatureThe mixture was heated
  2. customThe cooled reaction mixture
  3. concentrationwas concentrated in vacuo

Sources & evidence

ORD record
ord-35e675605ff140e586f6af40a5d81bec
Source dataset
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05239075

Reaction notes

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