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Pyrazole → Trifluoroacetic acid

HRID 60878
Notes
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Reaction equation

HRID 60878 reaction equation
Br[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[C:9]([N:11]1[CH2:16][CH2:15][CH2:14][C@H:13]([CH3:17])[C@@H:12]1[CH2:18][NH:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][N:21]=1)=[O:10].[NH:30]1[CH:34]=[CH:33][CH:32]=[N:31]1.CN[C@H]1CCCC[C@@H]1NC.[C:45]([O-:48])([O-])=[O:46].[Cs+].[Cs+]>[Cu]I.O1CCOCC1>[CH3:17][C@H:13]1[CH2:14][CH2:15][CH2:16][N:11]([C:9]([C:3]2[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=2[N:30]2[CH:34]=[CH:33][CH:32]=[N:31]2)=[O:10])[C@H:12]1[CH2:18][NH:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][N:21]=1.[C:45]([OH:48])([C:26]([F:29])([F:28])[F:27])=[O:46]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 4

HCID 1048PyrazoleHCID 10796Cesium carbonateHCID 13822957(1S,2S)-(+)-N,N'-Dimethylcyclohexane-1,2-diamineHCID 131737147rac-cis-(2-Bromo-5-methylphenyl)(3-methyl-2-(((5-(trifluoromethyl)pyridin-2-yl)amino)methyl)piperidin-1-yl)methanone

Product 2

HCID 6422Trifluoroacetic acid
HCID 131737158
rac-cis-(3-Methyl-2-(((5-(trifluoromethyl)pyridin-2-yl)amino)methyl)piperidin-1-yl)(5-methyl-2-(1H-pyrazol-1-yl)phenyl)methanone

Reagents, catalysts & solvents 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)CatalystHCID 312751,4-DioxaneSolvent

Conditions

Temperature
140 °C

Procedure

A mixture of rac-cis-(2-bromo-5-methylphenyl)(3-methyl-2-(((5-(trifluoromethyl)pyridin-2-yl)amino)methyl)piperidin-1-yl)methanone (0.0326 g, 0.0693 mmol), pyrazole (0.0094 g, 0.139 mmol), (1S,2S)—N1,N2-dimethylcyclohexane-1,2-diamine (0.004 g, 0.0277 mmol), Cs2CO3 (0.045 g, 0.139 mmol) and CuI (0.003 g, 0.0139 mmol) and dioxane (1.0 mL) was degassed and heated overnight at 140° C. The reaction was cooled to RT, and acidified with TFA to pH4-5. The solvent was removed in vacuo to obtain the crude which as purified by preparative-HPLC to obtain the title compound as a TFA salt. ESI-MS (m/z): 458, [M+1]+.

Workup

  1. customwas degassed
  2. temperatureThe reaction was cooled to RT
  3. customThe solvent was removed in vacuo
  4. customto obtain the crude which
  5. customas purified by preparative-HPLC

Sources & evidence

ORD record
ord-d415d17ca0894f4dbc2272ab40ff4ae9
Source dataset
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09440982B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes