Nitrogen → HCID 87486423, compound

HRID 1723857Notes

Reaction equation

HRID 1723857 reaction equation
[CH2:1]([S:7]([OH:10])(=[O:9])=[O:8])[CH2:2][S:3]([OH:6])(=[O:5])=[O:4].[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.C(OC)(C)(C)C>CO>[S:3]([CH2:2][CH2:1][S:7]([OH:10])(=[O:9])=[O:8])([OH:6])(=[O:5])=[O:4].[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

6

Reactant 4

HCID 947NitrogenHCID 80321,2-Ethanedisulfonic AcidHCID 15413tert-Butyl methyl etherHCID 11510935HCID 11510935, compound

Product 1

HCID 87486423HCID 87486423, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3.145 mg of ethanedisulfonic acid was added to 0.56 ml of a solution of 1-(2-fluorophenyl)-3-(piperidin-4-yloxy)-1H-indazole in MeOH (methanol) (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 (methyl tert-butyl ether) 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-83e93c68a173486286c805871e989d32
Source dataset
uspto-grants-2009_02
Patent number
US07485636B2

Reaction notes

Loading…