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1-Chloromethylnaphthalene → (2S,3S)-2-benzyloxy-5-(1-naphthyl)pentan-3-ol

HRID 278482
Notes
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Reaction equation

HRID 278482 reaction equation
[Mg:1].Cl[CH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1.[Cl-:14].[Li+].[CH2:16]([O:23][C@@H:24]([CH3:28])[CH:25]1[O:27][CH2:26]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>CCOCC.C1COCC1.[Cu](Cl)Cl.C(OCC)(=O)C.CCCCCC>[C:4]1([CH2:3][Mg:1][Cl:14])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1.[CH2:16]([O:23][C@H:24]([C@@H:25]([OH:27])[CH2:26][CH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1)[CH3:28])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[CH2:16]([O:23][C@H:24]([C@H:25]([OH:27])[CH2:26][CH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1)[CH3:28])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

12

Reactant 4

HCID 68451-ChloromethylnaphthaleneHCID 433294Lithium ChlorideHCID 5462224MagnesiumHCID 57223577(3S)-3-benzyloxy-1,2-epoxybutane

Product 3

HCID 57094200(2S,3S)-2-benzyloxy-5-(1-naphthyl)pentan-3-olYield 42%HCID 57321321
(2s,3r)-2-Benzyloxy-5-(1-naphthyl)pentan-3-ol
Yield 21.5%
HCID 178478993HCID 178478993, compound

Reagents, catalysts & solvents 5

HCID 24014Cupric ChlorideCatalystHCID 3283Diethyl EtherSolvent2×HCID 8028TetrahydrofuranSolventHCID 8058HexaneSolventHCID 8857Ethyl AcetateSolvent

Conditions

Temperature
-78 °C

Procedure

1-Naphthylmethylmagnesium chloride was prepared from magnesium turnings (2.88 g) and 1-(chloromethyl)naphthalene (6.98 g) in ether (80 ml) by the method of J. Am. Chem. Soc. (1943) 65, 295. A solution of lithium chloride (167 mg) and copper (II) chloride (266 mg) in THF (10 ml) was added dropwise to the ethereal solution of the Grignard reagent followed by addition of a solution of (2RS,3S)-3-(benzyloxy)-1,2-epoxybutane (3.52 g) in ether (30 ml) below −70° C. The mixture was stirred at −78° C. for 1 h, and then allowed to warm to room temperature and stirred overnight. After cooling, the mixture was quenched with saturated aqueous ammonium chloride solution (100 ml). The insoluble material was filtered through Celite and the filter cake was washed with ether. The filtrate and washings were combined, and the organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give an oil. Flash chromatography (hexane:ethyl acetate=9:1→4:1) gave (2S,3S)-2-benzyloxy-5-(1-naphthyl)pentan-3-ol (2.66 g, 42.0%) as the first eluate and (2S,3R)-2-benzyloxy-5-(1-naphthyl)pentan-3-ol (1.36 g, 21.5%) as the second eluate.

Workup

  1. temperatureto warm to room temperature
  2. stirringstirred overnight
  3. temperatureAfter cooling
  4. customthe mixture was quenched with saturated aqueous ammonium chloride solution (100 ml)
  5. filtrationThe insoluble material was filtered through Celite
  6. washthe filter cake was washed with ether
  7. washthe organic layer was washed with water and brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated in vacuo
  10. customto give an oil

Sources & evidence

ORD record
ord-17d3276a41c945ab91fb3a8d531442d6
Source dataset
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06359145B1

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes