Sulfuric Acid → HCID 21276171, compound

HRID 1381568Notes

Reaction equation

HRID 1381568 reaction equation
CO[CH:3](OC)[CH2:4][CH:5](OC)OC.S(=O)(=O)(O)O.[NH:17]([C:19]1[N:23]([C:24]2[C:29]([Cl:30])=[CH:28][C:27]([C:31]([F:34])([F:33])[F:32])=[CH:26][C:25]=2[Cl:35])[N:22]=[CH:21][C:20]=1[S:36]([C:39]([F:42])([F:41])[F:40])(=[O:38])=[O:37])[NH2:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Cl:30][C:29]1[CH:28]=[C:27]([C:31]([F:32])([F:33])[F:34])[CH:26]=[C:25]([Cl:35])[C:24]=1[N:23]1[C:19]([N:17]2[CH:5]=[CH:4][CH:3]=[N:18]2)=[C:20]([S:36]([C:39]([F:42])([F:41])[F:40])(=[O:37])=[O:38])[CH:21]=[N:22]1

Participants

6

Reactant 4

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 66019TetramethoxypropaneHCID 14032813HCID 14032813, compound

Product 1

HCID 21276171HCID 21276171, compoundYield 77%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.2 ml (0.0078 mole) of 1,1,3,3-tetramethoxypropane and 0.2 ml (0.0034 mole) of 96 percent strength sulphuric acid are added in sequence to 3 g (0.0068 mole) of 5-hydrazino-4-(trifluoromethylsulphonyl)-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole in 7 ml of ethanol at 20° C. to 25° C. The reaction mixture is heated at the reflux temperature for 2 hours, cooled, and neutralized with 0.36 g (0.0034 mole) of sodium carbonate, and the solvent is removed in vacuo. The residue is suspended in water, filtered, washed again with water and dried. 2.5 g (77% of theory) of 1-(2,6-dichloro-4-trifluoromethyl-phenyl)-5-(pyrazol-1-yl)-4-trifluoromethylsulphonyl-pyrazole of melting point 127° C. to 133° C. are obtained.

Workup

  1. temperatureThe reaction mixture is heated at the reflux temperature for 2 hours
  2. temperaturecooled
  3. customthe solvent is removed in vacuo
  4. filtrationfiltered
  5. washwashed again with water
  6. customdried

Sources & evidence

ORD record
ord-4997d4c5779449a4ba4c11d69d70bcb6
Source dataset
uspto-grants-1989_02
Patent number
US04803215

Reaction notes

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