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Allyl bromide → (2S,5R)-tert-Butyl 6-(allyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carboxylate

HRID 925142
Notes
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Reaction equation

HRID 925142 reaction equation
[CH2:1]([O:8][N:9]1[C:15](=[O:16])[N:14]2[CH2:17][C@H:10]1[CH2:11][CH2:12][C@H:13]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:2]1C=CC=C[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].C(Br)C=C>C(O)C.C(#N)C.[C].[Pd]>[CH2:1]([O:8][N:9]1[C:15](=[O:16])[N:14]2[CH2:17][C@H:10]1[CH2:11][CH2:12][C@H:13]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH:2]=[CH2:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 57389353(2S,5R)-tert-butyl 6-(benzyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carboxylate

Product 1

HCID 57389440(2S,5R)-tert-Butyl 6-(allyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carboxylateYield 54%

Reagents, catalysts & solvents 3

HCID 178418390
HCID 178418390, compound
Catalyst
HCID 702EthanolSolvent
HCID 6342AcetonitrileSolvent

Procedure

140 mg (0.421 mmol) of (2S,5R)-tert-butyl 6-(benzyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carboxylate was dissolved in ethanol (3.1 mL), and 14 mg of 10% palladium-carbon (50% water content) was added, followed by stirring at room temperature for 1 hour under hydrogen atmosphere. The catalyst of the reaction mixture was filtered through celite, and the residue resulting from concentration of the solvent under reduced pressure was dissolved in acetonitrile (4.1 mL), and 62 mg (0.449 mmol) of anhydrous potassium carbonate and 70 μL (0.809 mmol) of allyl bromide were added, followed by stifling at room temperature for 3 hours. After the reaction mixture was concentrated under reduced pressure, the residue was diluted with ethyl acetate and washed sequentially with water, saturated aqueous ammonium chloride solution and saturated brine, subsequently the organic layer was dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The resulting residue was applied to silica gel column chromatography (n-hexane/ethyl acetate=5/2) to afford 60.8 mg of the title compound (yield 54%). Enantiomeric excess: 99.9% ee or more (CHIRALPAK AD-H, 4.6×150 mm, hexane/ethanol=2/1, UV 210 nm, flow rate 1 mL/min., retention time 4.8 min.).

Workup

  1. filtrationThe catalyst of the reaction mixture was filtered through celite
  2. customthe residue resulting from concentration of the solvent under reduced pressure
  3. waitby stifling at room temperature for 3 hours
  4. concentrationAfter the reaction mixture was concentrated under reduced pressure
  5. additionthe residue was diluted with ethyl acetate
  6. washwashed sequentially with water, saturated aqueous ammonium chloride solution and saturated brine
  7. dry with materialsubsequently the organic layer was dried over anhydrous magnesium sulfate
  8. concentrationthe solvent was concentrated under reduced pressure

Sources & evidence

ORD record
ord-372c09a769fc4d788d4ea214a7401c17
Source dataset
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09284273B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes