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

HRID 1395436Notes

Reaction equation

HRID 1395436 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-e11c5ad23858493da8fce1e5c3a7c727
Source dataset
uspto-grants-1980_05
Patent number
US04203985

Reaction notes

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