Methanesulfonic Acid → HCID 86625065, compound

HRID 13787Notes

Reaction equation

HRID 13787 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:37]=[CH:36][C:12]([C:13]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([CH3:22])=[C:18]([NH:23][C:24]4[CH:29]=[C:28]([C:30]5[CH:31]=[N:32][CH:33]=[CH:34][CH:35]=5)[CH:27]=[CH:26][N:25]=4)[CH:17]=3)=[O:14])=[CH:11][C:10]=2[C:38]([F:41])([F:40])[F:39])[CH2:4][CH2:3]1.[CH3:42][S:43]([OH:46])(=[O:45])=[O:44]>CO>[CH3:42][S:43]([OH:46])(=[O:45])=[O:44].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:37]=[CH:36][C:12]([C:13]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([CH3:22])=[C:18]([NH:23][C:24]4[CH:29]=[C:28]([C:30]5[CH:31]=[N:32][CH:33]=[CH:34][CH:35]=5)[CH:27]=[CH:26][N:25]=4)[CH:17]=3)=[O:14])=[CH:11][C:10]=2[C:38]([F:41])([F:40])[F:39])[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 113075064-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-{4-methyl-3-[4-(3-pyridyl)pyridin-2-ylamino]phenyl}benzamide

Product 1

HCID 86625065HCID 86625065, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1.21 g of 4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-{4-methyl-3-[4-(3-pyridyl)pyridin-2-ylamino]phenyl}benzamide (Example 28) was suspended in 20 ml of methanol and 140 μl of methanesulfonic acid was added, followed by stirring with heating. Insolubles were removed by filtration with heating and the solvent in the filtrate was distilled off under reduced pressure. The residue was crystallized by adding isopropanol and collected by filtration to obtain 1.33 g of the objective compound as pale yellow crystals.

Workup

  1. temperaturewith heating
  2. customInsolubles were removed by filtration
  3. temperaturewith heating
  4. distillationthe solvent in the filtrate was distilled off under reduced pressure
  5. customThe residue was crystallized
  6. additionby adding isopropanol
  7. filtrationcollected by filtration

Sources & evidence

ORD record
ord-1e1e5b74926d46f2b263519345622ac9
Source dataset
uspto-grants-2010_06
Patent number
US07728131B2

Reaction notes

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