Trichloroisocyanuric Acid → HCID 68963317, compound

HRID 1396563Notes

Reaction equation

HRID 1396563 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:17]3[C:12](=[N:13][C:14]([NH2:18])=[N:15][CH:16]=3)[N:11]([CH3:19])[N:10]=2)=[CH:5][C:4]=1[C:20]([F:23])([F:22])[F:21].[Cl:24]N1C(=O)N(Cl)C(=O)N(Cl)C1=O>S(=O)(=O)(O)O>[Cl:24][C:8]1[CH:7]=[C:6]([C:9]2[C:17]3[C:12](=[N:13][C:14]([NH2:18])=[N:15][CH:16]=3)[N:11]([CH3:19])[N:10]=2)[CH:5]=[C:4]([C:20]([F:21])([F:23])[F:22])[C:3]=1[O:2][CH3:1]

Participants

4

Reactant 2

HCID 6909Trichloroisocyanuric AcidHCID 68962991HCID 68962991, compound

Product 1

HCID 68963317HCID 68963317, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

3-(4-Methoxy-3-trifluoromethyl-phenyl)-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-6-ylamine (Example 111, step 1) (182 mg, 0.56 mmol) is dissolved in concentrated sulfuric acid (11 ml) to give a red solution. Trichloroisocyanuric acid (44 mg, 0.188 mmol) is added and the reaction mixture is stirred at room temperature overnight then poured onto ice-water. After stirring for 30 minutes, the resulting precipitate is collected by filtration, washed with water and dried under vacuum (45°) to afford the title compound as the sulfate salt.

Workup

  1. customto give a red solution
  2. additionthen poured onto ice-water
  3. stirringAfter stirring for 30 minutes
  4. filtrationthe resulting precipitate is collected by filtration
  5. washwashed with water
  6. customdried under vacuum (45°)

Sources & evidence

ORD record
ord-d2b099d5b0e44c788bfafd8455abeead
Source dataset
uspto-grants-2014_12
Patent number
US08901134B2

Reaction notes

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