Sodium → HCID 135762629, compound

HRID 1076535Notes

Reaction equation

HRID 1076535 reaction equation
[Na].[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[O:12][C:13]3[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=3[C:15](=O)[N:16]=2)=[CH:7][CH:6]=1)([O-:4])=[O:3].S(O)(O)(=O)=O.[C:27]([NH:30][C:31]([NH2:33])=[O:32])(=[NH:29])[NH2:28]>CO>[NH:30]([C:27]1[N:29]=[C:11]([C:8]2[CH:9]=[CH:10][C:5]([N+:2]([O-:4])=[O:3])=[CH:6][CH:7]=2)[N:16]=[C:15]([C:14]2[CH:18]=[CH:19][CH:20]=[CH:21][C:13]=2[OH:12])[N:28]=1)[C:31]([NH2:33])=[O:32]

Participants

5

Reactant 3

HCID 5360545SodiumHCID 14146191HCID 14146191, compoundHCID 178513044HCID 178513044, compound

Product 1

HCID 135762629HCID 135762629, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

A solution of 8.9 g (385 millimoles) of sodium in 400 ml of methanol is added dropwise, while stirring, to a suspension of 93.9 g (350 millimoles) of 2-(4-nitrophenyl)-4H-1,3-benzoxazin-4-one and 58.1 g (192.5 millimoles) of guanyl urea sulfate in 1 liter of methanol. Subsequently, the mixture is refluxed for 30 minutes. After cooling of the mixture, the precipitate formed is suction-filtered, washed with water and methanol and dried at 70°C in a vacuum drying oven. The yield is 61.9 g (50.2 % of the theoretical yield). The 4-ureido-2-(2-hydroxyphenyl)-6-(4-nitrophenyl)-s-triazine obtained is a powder having a light yellow color and a melting point of 249°C (decomposition).

Workup

  1. temperatureSubsequently, the mixture is refluxed for 30 minutes
  2. temperatureAfter cooling of the mixture
  3. customthe precipitate formed
  4. filtrationis suction-filtered
  5. washwashed with water and methanol
  6. customdried at 70°C in a vacuum
  7. customdrying oven
  8. customThe yield is 61.9 g (50.2 % of the theoretical yield)

Sources & evidence

ORD record
ord-1989ef863ecf4cd7bdf717dd18f4bcc8
Source dataset
uspto-grants-1976_05
Patent number
US03957780

Reaction notes

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