Carbon Dioxide → HCID 57034955, compound

HRID 544521Notes

Reaction equation

HRID 544521 reaction equation
S(=O)(=O)(O)O.Cl.C([CH:9]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=1)[C:10](=[O:17])[CH2:11][N:12]1[CH:16]=[N:15][CH:14]=[N:13]1)#N.C(=O)=O>O>[F:26][C:24]([F:25])([F:27])[C:20]1[CH:19]=[C:18]([CH2:9][C:10](=[O:17])[CH2:11][N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[CH:23]=[CH:22][CH:21]=1

Participants

5

Reactant 3

HCID 280Carbon DioxideHCID 1118Sulfuric AcidHCID 86739431HCID 86739431, compound

Product 1

HCID 57034955HCID 57034955, compoundYield 72%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
100 °C

Procedure

320 ml of concentrated sulphuric acid and 94 ml of water were added to 266.3 g of 1-cyano-1-(3-trifluoromethylphenyl)-3-(1,2,4-triazol-l-yl)-propanone hydrochloride, and the mixture was heated at 100° C. for 1.5 hours. After the vigorous evolution of CO2 had ended, the mixture was allowed to cool, and 940 ml of water were added. After a short time at from 0° to 20° C., the sulphate of the desired end product crystallized out. This was suspended in water, and the suspension was adjusted to a pH value of 7-8 with sodium bicarbonate solution. The resulting crystalline precipitate was filtered off under suction, dissolved in chloroform, dried over sodium sulphate and concentrated. 131.3 g (72% of theory) of 1-(3-trifluoromethylphenyl)-3-(1,2,4-triazol-l-yl)-propanone of melting point 85° to 87° C. were obtained. ##STR8##

Workup

  1. temperatureto cool
  2. customAfter a short time at from 0° to 20° C., the sulphate of the desired end product crystallized out
  3. filtrationThe resulting crystalline precipitate was filtered off under suction
  4. dissolutiondissolved in chloroform
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-e18c4cfaf2f04316860703fdbb387048
Source dataset
uspto-grants-1984_05
Patent number
US04451282

Reaction notes

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