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HCID 21104706, compound → HCID 21104576, compound

HRID 1354233
Notes
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Reaction equation

HRID 1354233 reaction equation
[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][NH:12][CH2:13][C:14]3[CH2:19][N:18](NC(OC(C)(C)C)=O)[CH2:17][CH2:16][CH:15]=3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1>C(O)(C(F)(F)F)=O>[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][NH:12][CH2:13][C:14]3[CH2:19][NH:18][CH2:17][CH2:16][CH:15]=3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 21104706HCID 21104706, compound

Product 1

HCID 21104576HCID 21104576, compound

Reagents, catalysts & solvents 1

HCID 6422Trifluoroacetic acidSolvent

Procedure

A solution of tert-butyl 5-{[(2,3-dihydro-benzo[1,4]-dioxin-6-ylmethyl)-amino]-methyl}-3,6-dihydro-2H-pyridine-1-carbamate (0.16 g, 0.44 mmol) in TFA (3 ml) was stirred at room temperature for 30 minutes, concentrated and taken up in saturated bicarbonate solution (30 ml) and dichloromethane (30 ml). The aqueous phase was extracted with dichloromethane (2×30 ml) and the combined organic phases were washed with saturated sodium chloride solution, dried over MgSO4 and concentrated.

Workup

  1. concentrationconcentrated
  2. extractionThe aqueous phase was extracted with dichloromethane (2×30 ml)
  • washthe combined organic phases were washed with saturated sodium chloride solution
  • dry with materialdried over MgSO4
  • concentrationconcentrated
  • Sources & evidence

    ORD record
    ord-7451420421c046709b49d608bad220da
    Source dataset
    uspto-grants-2007_05
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US07223776B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes