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

HRID 1395424Notes

Reaction equation

HRID 1395424 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 EtOH 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 EtOH

Sources & evidence

ORD record
ord-d4cf400711cf49faa133fdbf947d7f81
Source dataset
uspto-grants-1980_05
Patent number
US04203983

Reaction notes

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