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Methylamine → 4'-(Methylamino)spiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyridine]

HRID 48528
Notes
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Reaction equation

HRID 48528 reaction equation
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[O:8][C:9]3([CH:15]4[CH2:16][CH2:17][N:12]([CH2:13][CH2:14]4)[CH2:11]3)[CH2:10][C:3]=12.[CH3:18][NH2:19]>>[CH3:18][NH:19][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[O:8][C:9]3([CH:15]4[CH2:16][CH2:17][N:12]([CH2:13][CH2:14]4)[CH2:11]3)[CH2:10][C:3]=12
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 6329MethylamineHCID 100377734'-chlorospiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyridine]

Product 1

HCID 220458494'-(Methylamino)spiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyridine]

Procedure

A solution of 151 mg (0.60 mmol) of 4′-chlorospiro[1-azabicyclo[2.2.2]octane-3,2′(3′H)-furo[2,3-b]pyridine] in 25 mL of 40% aqueous methylamine was heated to 175° C. in a steel bomb for 18 hours, then cooled to ambient temperature and concentrated in vacuo. The residue was dissolved in 10 mL of ethanol containing 0.4 mL of concentrated hydrochloric acid and the solution was allowed to stand overnight. After filtering, the solution was concentrated in vacuo and the residue crystallized from isopropanol, giving 147 mg of the title compound as a white solid: electrospray MS (m/z, relative intensity) 246 ([MH]+).

Workup

  • concentrationconcentrated in vacuo
  • dissolutionThe residue was dissolved in 10 mL of ethanol containing 0.4 mL of concentrated hydrochloric acid
  • filtrationAfter filtering
  • concentrationthe solution was concentrated in vacuo
  • customthe residue crystallized from isopropanol
  • Sources & evidence

    ORD record
    ord-63cfe256fd9c4cd887b1b4309f8a3ef8
    Source dataset
    uspto-grants-2004_03
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US06703502B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes