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Acetic Acid → 11-Allyl-6-methoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-8-one

HRID 272602
Notes
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Reaction equation

HRID 272602 reaction equation
O[CH:2]1[CH:8](O)[CH:7]2[CH2:10][CH:3]1[C:4]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[C:5]=1[C:6]2=[O:11].[C:18]([O-])(=O)[CH3:19].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4].CC(O)=O.[CH2:39]([NH2:42])C=C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+]>ClCCl>[CH2:39]([N:42]1[CH2:2][CH:3]2[CH2:10][CH:7]([C:6](=[O:11])[C:5]3[C:12]([O:16][CH3:17])=[CH:13][CH:14]=[CH:15][C:4]=32)[CH2:8]1)[CH:18]=[CH2:19]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 6

HCID 176Acetic AcidHCID 7853AllylamineHCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 598378516,7-Dihydroxy-1-methoxy-5,6,7,8-tetrahydro-5,8-methano-benzocyclohepten-9-oneHCID 178418268HCID 178418268, compound

Product 1

HCID 5983786311-Allyl-6-methoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-8-one

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

6,7-Dihydroxy-1-methoxy-5,6,7,8-tetrahydro-5,8-methano-benzocyclohepten-9-one (2.80 g, 12 mmol) was stirred at 0° C. in dichloromethane (15 mL) and treated with lead tetraacetate (Pb(OAc)4, 5.35 g, 12 mmol). After 30 min. the mixture was filtered through a Celite™ pad and rinsed with dichloromethane (50 mL). To the stirred filtrate was added AcOH (3.61 g, 60 mmol) and allyl amine (689 mg, 12 mmol). After 15 min., the mixture was treated with NaBH(OAc)3 (7.70 g, 36 mmol) and stirred for 18 h. The mixture was poured into a saturated aqueous Na2CO3 solution (100 mL) stirred for 30 min. The layers were separated and extracted with EtOAc (2×100 mL). The organic layer was washed with a saturated aqueous Na2CO3 solution (2×50 mL), H2O (50 mL), saturated aqueous NaCl solution (50 mL), dried over MgSO4, filtered and concentrated to an oil. Purification by chromatography on silica gel eluting with 5% EtOAc/hexanes provided product as an oil (885 mg, 29%). (TLC 30% EtOAc/hexanes Rf 0.67).

Workup

  1. filtrationAfter 30 min. the mixture was filtered through a Celite™ pad
  2. washrinsed with dichloromethane (50 mL)
  3. stirringstirred for 30 min
  4. customThe layers were separated
  5. extractionextracted with EtOAc (2×100 mL)
  6. washThe organic layer was washed with a saturated aqueous Na2CO3 solution (2×50 mL), H2O (50 mL), saturated aqueous NaCl solution (50 mL)
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated to an oil
  10. customPurification by chromatography on silica gel eluting with 5% EtOAc/hexanes provided product as an oil (885 mg, 29%)

Sources & evidence

ORD record
ord-de1932bdc7d549ae9694e0649e5f1e76
Source dataset
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07456177B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes