Potassium Carbonate → HCID 22480372, compound

HRID 1275716Notes

Reaction equation

HRID 1275716 reaction equation
P(Cl)(Cl)(Cl)=O.[CH2:6]([N:13]1[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][C:15]([C:22]2[O:23][CH:24]=[CH:25][CH:26]=2)=[N:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[C:27](=O)([O-])[O-:28].[K+].[K+]>CN(C=O)C>[CH2:6]([N:13]1[C:17]([C:18]([F:20])([F:21])[F:19])=[CH:16][C:15]([C:22]2[O:23][C:24]([CH:27]=[O:28])=[CH:25][CH:26]=2)=[N:14]1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 24813Phosphorus oxychlorideHCID 22480365HCID 22480365, compound

Product 1

HCID 22480372HCID 22480372, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent2×

Procedure

10 ml of dry DMF were initially charged at 10° C., 1.9 g (12.4 mmol) of phosphorus oxychloride were added dropwise and the mixture was stirred for 30 min. A solution of 3 g (10.3 mmol) of 1-benzyl-3-(2-furyl)-5-trifluoromethylpyrazole in 10 ml of DMF was added dropwise, and the mixture was stirred at RT overnight. The mixture was poured into ice-water and adjusted to pH 9 using potassium carbonate solution. The precipitated product was filtered off with suction and dried in a vacuum drying cabinet at 50° C. This gave 3.3 g (100%) of the title compound. m.p.: 76.5-77.5° C.

Workup

  1. stirringthe mixture was stirred at RT overnight
  2. filtrationThe precipitated product was filtered off with suction
  3. customdried in a vacuum
  4. customdrying cabinet at 50° C

Sources & evidence

ORD record
ord-f991cf4bed9444fab36785598c5e81e0
Source dataset
uspto-grants-2000_12
Patent number
US06162819

Reaction notes

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