Methanesulfonic Acid → 4-[(4-Methylpiperazin-1-yl)methyl]-n-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid salt

HRID 1926593Notes

Reaction equation

HRID 1926593 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:17]=[N:18][C:19]([CH3:35])=[C:20]([NH:22][C:23]4[N:28]=[C:27]([C:29]5[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=5)[CH:26]=[CH:25][N:24]=4)[CH:21]=3)=[O:14])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>>[CH3:38][S:39]([OH:42])(=[O:41])=[O:40].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([C:13]([NH:15][C:16]3[CH:17]=[N:18][C:19]([CH3:35])=[C:20]([NH:22][C:23]4[N:28]=[C:27]([C:29]5[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=5)[CH:26]=[CH:25][N:24]=4)[CH:21]=3)=[O:14])=[CH:36][CH:37]=2)[CH2:4][CH2:3]1

Participants

3

Reactant 2

HCID 6395Methanesulfonic AcidHCID 692278004-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide

Product 1

HCID 877440834-[(4-Methylpiperazin-1-yl)methyl]-n-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid saltYield 92.1%

Procedure

To a flask was added 4-[(4-methylpiperazin-1-yl) methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide (2.0 g), methanesulfonic acid (0.40 g) and purified water (100 mL). After the solution was clear, the reaction mixture was filtrated and the filtrate was freeze-dried to give 4-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid salt (2.2 g).

Workup

  1. custompurified water (100 mL)
  2. filtrationthe reaction mixture was filtrated
  3. customthe filtrate was freeze-dried

Sources & evidence

ORD record
ord-20dfd9a39f134cd1929600576611a31d
Source dataset
uspto-grants-2012_05
Patent number
US08183242B2

Reaction notes

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