HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

1-Hydroxybenzotriazole → N-biphenyl-4-yl-3-[4-(2-chloro-5-fluoro-phenoxy)-piperidin-1-yl]-3-oxo-propionamide

HRID 1093668
Notes
Print preview

Reaction equation

HRID 1093668 reaction equation
[C:1]1([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:6]=[CH:5][C:4]([NH:7][C:8](=[O:13])[CH2:9][C:10]([OH:12])=O)=[CH:3][CH:2]=1.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.Cl.Cl.[Cl:52][C:53]1[CH:65]=[CH:64][C:63]([F:66])=[CH:62][C:54]=1[O:55][CH:56]1[CH2:61][CH2:60][NH:59][CH2:58][CH2:57]1>CN(C=O)C.O>[C:1]1([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:2]=[CH:3][C:4]([NH:7][C:8](=[O:13])[CH2:9][C:10]([N:59]2[CH2:58][CH2:57][CH:56]([O:55][C:54]3[CH:62]=[C:63]([F:66])[CH:64]=[CH:65][C:53]=3[Cl:52])[CH2:61][CH2:60]2)=[O:12])=[CH:5][CH:6]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 167327404-(2-Chloro-5-fluoro-phenoxy)-piperidine hydrochlorideHCID 55049154N-biphenyl-4-yl-malonamic acid

Product 1

HCID 57874507
N-biphenyl-4-yl-3-[4-(2-chloro-5-fluoro-phenoxy)-piperidin-1-yl]-3-oxo-propionamide
Yield 13.2%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6228DimethylformamideSolvent

Conditions

Temperature
10 °C

Procedure

To a stirred solution of N-biphenyl-4-yl-malonamic acid (0.1 g, 0.00039 mole) in DMF (2 mL) was added HOBt (0.065 g, 0.00047 mole) and DIPEA (0.126 g, 0.00098 mole). The mixture was cooled to 10° C. and EDCI.HCl (0.090 g, 0.00047 mole) followed by 4-(2-chloro-5-fluoro-phenoxy)-piperidine hydrochloride (0.114 g, 0.00043 mole) were added. The resulting mixture was stirred at the ambient temperature overnight. The mixture was then diluted with cold water and the resulting precipitate was isolated by filtration. Purification by column chromatography using silica gel 60-120 mesh (35% ethyl acetate in hexane) afforded 0.024 g (13%) of N-biphenyl-4-yl-3-[4-(2-chloro-5-fluoro-phenoxy)-piperidin-1-yl]-3-oxo-propionamide. LCMS: 467 (M+1)+, 97.5%, 1H NMR (CDCl3): δ 10.0 (s, 1H), 7.66 (d, 2H), 7.58 (m, 4H), 7.42 (t, 2H), 7.34 (m, 2H), 6.68 (m, 2H), 4.64 (m, 1H), 4.3 (m, 1H), 3.7 (m, 3H), 3.52 (s, 2H), 1.96 (m, 4H).

Workup

  1. additionwere added
  2. customthe resulting precipitate was isolated by filtration
  3. customPurification by column chromatography

Sources & evidence

ORD record
ord-188383c60ccb4d9c96b5b17343b5cf36
Source dataset
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08129376B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes