Nitrogen → HCID 11510934, compound

HRID 1723856Notes

Reaction equation

HRID 1723856 reaction equation
[C:1]([OH:10])(=[O:9])[C@@H:2]([C@H:4]([C:6]([OH:8])=[O:7])[OH:5])[OH:3].[F:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N:18]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:20]([O:27][CH:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)=[N:19]1.N#N>CO>[C:6]([C@@H:4]([C@H:2]([C:1]([OH:10])=[O:9])[OH:3])[OH:5])([OH:8])=[O:7].[F:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N:18]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:20]([O:27][CH:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)=[N:19]1

Participants

5

Reactant 3

HCID 947NitrogenHCID 444305L-Tartaric acidHCID 11510935HCID 11510935, compound

Product 1

HCID 11510934HCID 11510934, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

65.9 mg of L-tartaric acid was added to 136.68 mg of 1-(2-fluorophenyl)-3-(piperidin-4-yloxy)-1H-indazole (clear oil) in 12.45 ml of methanol. The mixture was place under a stream of N2 gas until only approximately 1 ml of solution remained. Precipitation of the salt was observed during this step. Approximately 5 ml of acetone was added and the subsequent solution was then stirred briefly (˜2 min). A white solid was recovered using vacuum filtration with a membrane filter. The solid was dried in a vacuum dessicator at ambient temperature (pressure not controlled).

Workup

  1. customPrecipitation of the salt
  2. additionApproximately 5 ml of acetone was added
  3. customA white solid was recovered
  4. filtrationvacuum filtration with a membrane
  5. filtrationfilter
  6. customThe solid was dried in a vacuum dessicator at ambient temperature (pressure not

Sources & evidence

ORD record
ord-250507405c0044758b33e6f2006a80fc
Source dataset
uspto-grants-2009_02
Patent number
US07485636B2

Reaction notes

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