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Benzylamine → 11-(Phenylmethyl)-3,11-diazatricyclo[7.3.1.02,7]trideca-2,4,6-triene

HRID 1727183
Notes
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Reaction equation

HRID 1727183 reaction equation
[CH:1]12[CH2:14][CH:9]([CH:10](O)[CH:11]1O)[CH2:8][C:7]1[C:2]2=[N:3][CH:4]=[CH:5][CH:6]=1.I([O-])(=O)(=O)=O.[Na+].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C(O)C.O.ClC(Cl)C.C(OCC)(=O)C>[C:22]1([CH2:21][N:28]2[CH2:11][CH:1]3[CH2:14][CH:9]([CH2:8][C:7]4[C:2]3=[N:3][CH:4]=[CH:5][CH:6]=4)[CH2:10]2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

10

Reactant 5

HCID 7504BenzylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 23667635Sodium periodateHCID 688083706,7,8,9-Tetrahydro-5H-6,9-methanocyclohepta[b]pyridine-7,8-diol

Product 1

HCID 59837841
11-(Phenylmethyl)-3,11-diazatricyclo[7.3.1.02,7]trideca-2,4,6-triene
Yield 50%

Reagents, catalysts & solvents 4

HCID 702EthanolSolventHCID 962WaterSolvent2×HCID 63651,1-DichloroethaneSolventHCID 8857Ethyl AcetateSolvent2×

Procedure

To a solution of 3-azatricyclo[7.2.1.02,7]dodeca-2,4,6-triene-10,11-diol (Preparation 24, 1.16 g, 6.07 mmol) in ethanol (40 ml) was added sodium periodate (1.35 g, 6.07 mmol) in water (20 ml) to produce a yellow slurry. After 15 min, water and ethyl acetate were added and the layers were separated, the aqueous layer washed with ethyl acetate (4×50 ml) and then dichloromethane. The combined organic extracts were dried (Na2SO4) to give an orange oil. The oil was diluted with dichloroethane (50 ml), benzylamine (0.65 g, 6.07 mmol) was added followed by sodium triacetoxyborohydride (4.12 g, 19.4 mmol). After 7 h, saturated sodium hydrogen carbonate solution (75 ml) and ethyl acetate (75 ml) were added and the reaction mixture was stirred for 20 min. The layers were separated and the aqueous layer was extracted with ethyl acetate (2×50 ml). The combined organic extracts were washed with water and brine, and then dried (Na2SO4) and concentrated in vacuo to give the crude product. Purification by flash chromatography produced the title compound as a light yellow oil (0.80 g, 50%).

Workup

  1. customto produce a yellow slurry
  2. customthe layers were separated
  3. washthe aqueous layer washed with ethyl acetate (4×50 ml)
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. customto give an orange oil
  6. additionwas added
  7. waitAfter 7 h
  8. customThe layers were separated
  9. extractionthe aqueous layer was extracted with ethyl acetate (2×50 ml)
  10. washThe combined organic extracts were washed with water and brine
  11. dry with materialdried (Na2SO4)
  12. concentrationconcentrated in vacuo
  13. customto give the crude product
  14. customPurification by flash chromatography

Sources & evidence

ORD record
ord-86e926c912d34b0bae22a3115bbc3bf3
Source dataset
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07494992B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes