Methanesulfonic Acid → HCID 86752728, compound

HRID 963439Notes

Reaction equation

HRID 963439 reaction equation
[CH3:1][N:2]([CH3:43])[CH2:3][CH2:4][CH2:5][NH:6][C:7]([C:9]1[C:18](=[O:19])[C:17]2[C:12](=[CH:13][C:14]([C:20]#[C:21][C:22]3[CH:27]=[C:26]([CH2:28][C:29]4[C:30]([NH2:36])=[N:31][C:32]([NH2:35])=[N:33][CH:34]=4)[CH:25]=[C:24]([O:37][CH3:38])[C:23]=3[O:39][CH3:40])=[CH:15][CH:16]=2)[N:11]([CH2:41][CH3:42])[CH:10]=1)=[O:8].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46]>O>[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:43][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][NH:6][C:7]([C:9]1[C:18](=[O:19])[C:17]2[C:12](=[CH:13][C:14]([C:20]#[C:21][C:22]3[CH:27]=[C:26]([CH2:28][C:29]4[C:30]([NH2:36])=[N:31][C:32]([NH2:35])=[N:33][CH:34]=4)[CH:25]=[C:24]([O:37][CH3:38])[C:23]=3[O:39][CH3:40])=[CH:15][CH:16]=2)[N:11]([CH2:41][CH3:42])[CH:10]=1)=[O:8]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 57176132HCID 57176132, compound

Product 1

HCID 86752728HCID 86752728, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A suspension of 0.2 g of 1-ethyl-7-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3-dimethoxy-phenylethynyl]-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (3-dimethylamino-propyl)-amide (Example 12z)) in 50 ml-of water is treated with a 0.1N aqueous methanesulphonic acid solution, with a slightly turbid solution being obtained. This solution is filtered and the filtrate is lyophilized. 1-ethyl-7-[5-(2,4-diamino-pyrimidin-5-yl-methyl)-2,3-dimethoxy-phenylethynyl]-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (3-dimethylamino-propyl)-amide dimethanesulphonate are obtained as a yellowish amorphous solid. Mass spectrum (FAB): 584 (M++H).

Workup

  1. custombeing obtained
  2. filtrationThis solution is filtered

Sources & evidence

ORD record
ord-2bc29502d93a4c5c871c66d0a5ede39d
Source dataset
uspto-grants-1998_06
Patent number
US05763450

Reaction notes

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