Nitrogen → HCID 68531372, compound

HRID 1723858Notes

Reaction equation

HRID 1723858 reaction equation
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[F:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:18]([O:25][CH:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)=[N:17]1.N#N.CC(OC)(C)C>CO>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[F:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:18]([O:25][CH:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)=[N:17]1

Participants

6

Reactant 4

HCID 947NitrogenHCID 15413tert-Butyl methyl etherHCID 444972Fumaric AcidHCID 11510935HCID 11510935, compound

Product 1

HCID 68531372HCID 68531372, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

2.162 mg of fumaric acid was added to 0.58 ml of a solution of 1-(2-fluorophenyl)-3-(piperidin-4-yloxy)-1H-indazole in MeOH (concentration=10.3 mg/ml). The solution was heated and stirred in uncapped vials and then placed under a stream of N2 gas. These steps were repeated until approximately 0.100 ml or less of solution remained. Approximately 0.500 ml of MTBE was then added. Precipitation was observed and the suspension was capped and stirred for 3 hours or less. The vial was then uncapped and allowed to stir for approximately 16 hours. A dry white solid remained.

Workup

  1. temperatureThe solution was heated
  2. customPrecipitation
  3. customthe suspension was capped
  4. stirringstirred for 3 hours or less
  5. stirringto stir for approximately 16 hours

Sources & evidence

ORD record
ord-46fcc80a859b4f1fa88794937a809f93
Source dataset
uspto-grants-2009_02
Patent number
US07485636B2

Reaction notes

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