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Triethylamine → N-[(3R)-6-(4-Hydroxyphenyl)-2-oxoazepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide

HRID 20155
Notes
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Reaction equation

HRID 20155 reaction equation
C(N(CC)CC)C.[NH2:8][C@@H:9]1[CH2:15][CH2:14][CH:13]([C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[CH2:12][NH:11][C:10]1=[O:23].Cl[C:25](OC1C=CC([N+]([O-])=O)=CC=1)=[O:26].Cl.Cl.[O:39]=[C:40]1[NH:48][C:43]2=[N:44][CH:45]=[CH:46][CH:47]=[C:42]2[N:41]1[CH:49]1[CH2:54][CH2:53][NH:52][CH2:51][CH2:50]1.C(N(C(C)C)CC)(C)C>CN(C)C=O.O1CCCC1>[OH:22][C:19]1[CH:20]=[CH:21][C:16]([CH:13]2[CH2:12][NH:11][C:10](=[O:23])[C@H:9]([NH:8][C:25]([N:52]3[CH2:53][CH2:54][CH:49]([N:41]4[C:42]5[C:43](=[N:44][CH:45]=[CH:46][CH:47]=5)[NH:48][C:40]4=[O:39])[CH2:50][CH2:51]3)=[O:26])[CH2:15][CH2:14]2)=[CH:17][CH:18]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 8471TriethylamineHCID 81531DiisopropylethylamineHCID 821294-Nitrophenyl chloroformateHCID 222931811-(piperidin-4-yl)-1H,2H,3H-imidazo[4,5-b]pyridin-2-one dihydrochlorideHCID 60037861(3R)-3-Amino-6-(4-hydroxyphenyl)azepan-2-one

Product 1

HCID 23656587
N-[(3R)-6-(4-Hydroxyphenyl)-2-oxoazepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide
Yield 33.5%

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8028TetrahydrofuranSolvent

Procedure

Triethylamine (0.009 mL, 0.091 mmol) was added to a solution of (3R)-3-amino-6-(4-hydroxyphenyl)azepan-2-one (10 mg, 0.045 mmol) and 4-nitrophenyl chloroformate (18 mg, 0.091 mmol) in N,N-dimethylformamide (0.2 mL) and tetrahydrofuran (0.2 mL) at 0° C. After 1 h, 2-oxo-1-(4-piperidinyl)-2,3-dihydro-1H-imidazo[4,5-b]pyridine dihydrochloride (26 mg, 0.091 mmol) and diisopropylethylamine (0.032 mL, 0.182 mmol) were added and the mixture was allowed to warm to ambient temperature. After 18 h, the mixture was purified by reverse phase HPLC (C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.1% trifluoroacetic acid) to give the title compound (7 mg). MS 465.2243 (M+1).

Workup

  1. waitAfter 18 h
  2. customthe mixture was purified by reverse phase HPLC (C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.1% trifluoroacetic acid)

Sources & evidence

ORD record
ord-3bc478f794524be086af371351a89b76
Source dataset
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07745427B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes