Methanesulfonic Acid → 1-(2',6'-Dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one methanesulfonate

HRID 2049545Notes

Reaction equation

HRID 2049545 reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH:14]=[N:13][CH:12]([NH:15][CH3:16])[NH:11][C:10]1=[O:17].[CH3:18][S:19]([OH:22])(=[O:21])=[O:20]>O>[CH3:18][S:19]([OH:22])(=[O:21])=[O:20].[CH3:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[C:3]=1[N:9]1[CH:14]=[N:13][C:12]([NH:15][CH3:16])=[N:11][C:10]1=[O:17]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 705842081-(2,6-Dimethylphenyl)-4-methylamino-dihydro-1,3,5-triazin-2-one

Product 1

HCID 204573291-(2',6'-Dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one methanesulfonateYield 94.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 6.0 g (0.026 moles) of 1-(2,6-dimethylphenyl)-4-methylamino-dihydro-1,3,5-triazin-2-one in 100 ml iPA was prepared with warming. To the warm solution was added 2.0 ml (0.031 moles) of methane-sulfonic acid. The mixture became hot and crystals of white crystalline solid began to form almost immediately. The mixture allowed to cool to room temperature in tap water and filtered. The solution was washed with IPA/Et2O to give 8.00 g of product which was dried overnight at 50°-60° C. in a vacuum. Obtained 8.0 g of 1-(2,6-dimethylphenyl)-4-methylaminodihydro-1,3,5-triazin-2-one methanesulfonate after drying.

Workup

  1. temperaturewith warming
  2. customto form almost immediately
  3. filtrationfiltered
  4. washThe solution was washed with IPA/Et2O

Sources & evidence

ORD record
ord-559d1ec059f54d56b696d876a7cb13a4
Source dataset
uspto-grants-1980_04
Patent number
US04198409

Reaction notes

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