Phosphate → HCID 19850697, compound

HRID 1607504Notes

Reaction equation

HRID 1607504 reaction equation
[Cl-].[NH2:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]=[N:10][C:11]2[CH:19]=[CH:18][C:14]([C:15]([NH2:17])=[NH2+:16])=[CH:13][CH:12]=2)=[C:5]([CH3:20])[CH:4]=1.[N:21]1[C:28]([Cl:29])=[N:27][C:25](Cl)=[N:24][C:22]=1[Cl:23].[OH-].[Na+].P([O-])([O-])([O-])=O>O>[Cl-:23].[Cl:23][C:22]1[N:21]=[C:28]([Cl:29])[N:27]=[C:25]([NH:2][C:3]2[CH:8]=[CH:7][C:6]([N:9]=[N:10][C:11]3[CH:12]=[CH:13][C:14]([C:15]([NH2:17])=[NH2+:16])=[CH:18][CH:19]=3)=[C:5]([CH3:20])[CH:4]=2)[N:24]=1

Participants

6

Reactant 4

HCID 1061PhosphateHCID 7954Cyanuric chlorideHCID 14798Sodium HydroxideHCID 19850695HCID 19850695, compound

Product 1

HCID 19850697HCID 19850697, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To an ice-cold solution of 5.8 g of 4-(4'-amino-2'-methylphenylazo)benzamidinium chloride in 800 parts of water was added 3.8 g of cyanuric chloride and the pH maintained between 5 and 6 and finally raised to 7 by the addition of 20 g of 1M sodium hydroxide solution. To this solution were then added 8 g of mixed phosphate buffer (equimolar amounts of KH2PO4 and Na2HPO4), followed by 40 g of salt and the precipitate of dichlorotriazine filtered off, mixed with further 1 g of phosphate buffer to ensure stability during drying and dried in vacuo giving 4-(4-[4,6-dichloro-s-triazin-2-ylamino]-2-methyl-phenylazo)benzamidinium chloride.

Workup

  1. temperaturethe pH maintained between 5 and 6
  2. filtrationthe precipitate of dichlorotriazine filtered off
  3. additionmixed with further 1 g of phosphate buffer
  4. customduring drying
  5. customdried in vacuo

Sources & evidence

ORD record
ord-3134012800f94f629429bbae53abbbed
Source dataset
uspto-grants-1989_09
Patent number
US04865990

Reaction notes

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