Methanesulfonic Acid → HCID 86615797, compound

HRID 1787069Notes

Reaction equation

HRID 1787069 reaction equation
[CH3:1][S:2]([CH2:5][C:6]([NH:8][CH2:9][CH2:10][N:11]1[C:19]2[C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([O:27][C:28]4[CH:33]=[CH:32][CH:31]=[C:30]([C:34]([F:37])([F:36])[F:35])[CH:29]=4)=[C:23]([CH3:38])[CH:22]=3)=[N:17][CH:16]=[N:15][C:14]=2[CH:13]=[CH:12]1)=[O:7])(=[O:4])=[O:3].[CH3:39][S:40]([OH:43])(=[O:42])=[O:41]>C(OCC)(=O)C>[CH3:39][S:40]([OH:43])(=[O:42])=[O:41].[CH3:1][S:2]([CH2:5][C:6]([NH:8][CH2:9][CH2:10][N:11]1[C:19]2[C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([O:27][C:28]4[CH:33]=[CH:32][CH:31]=[C:30]([C:34]([F:36])([F:37])[F:35])[CH:29]=4)=[C:23]([CH3:38])[CH:22]=3)=[N:17][CH:16]=[N:15][C:14]=2[CH:13]=[CH:12]1)=[O:7])(=[O:3])=[O:4]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 57597214HCID 57597214, compound

Product 1

HCID 86615797HCID 86615797, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

2-(Methylsulfonyl)-N-{2-[4-({3-methyl-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}acetamide (680 mg) was dissolved in ethyl acetate (3.4 mL), methanesulfonic acid (0.0887 mL) was added at 50° C., and the mixture was stirred for 10 min. and further stirred at room temperature for 2 hrs. The precipitated crystals were collected by filtration and washed with diisopropyl ether to give the title compound (797 mg) as colorless crystals.

Workup

  1. stirringfurther stirred at room temperature for 2 hrs
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed with diisopropyl ether

Sources & evidence

ORD record
ord-1206b0d56e3440eb8baf39b4de1476e3
Source dataset
uspto-grants-2009_03
Patent number
US07507740B2

Reaction notes

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