Peracetic Acid → HCID 178463106, compound

HRID 1275455Notes

Reaction equation

HRID 1275455 reaction equation
[CH2:1]([N:3]1[C:7]([OH:8])=[C:6]([C:9]([C:11]2[C:12]([CH3:23])=[C:13]3[C:18](=[C:19]([CH3:21])[CH:20]=2)S[CH:16]=[CH:15][C:14]3=[O:22])=[O:10])[CH:5]=[N:4]1)[CH3:2].C(OO)(=O)C.C(O)(=O)C.[S:33]([O-:36])([O-])=[O:34].[Na+].[Na+].C(OO)(=O)C>C(Cl)(Cl)Cl.O>[CH2:1]([N:3]1[C:7]([OH:8])=[C:6]([C:9]([C:11]2[C:12]([CH3:23])=[C:13]3[C:18](=[C:19]([CH3:21])[CH:20]=2)[S:33](=[O:36])(=[O:34])[CH:16]=[CH:15][C:14]3=[O:22])=[O:10])[CH:5]=[N:4]1)[CH3:2]

Participants

7

Reactant 4

HCID 6585Peracetic AcidHCID 24437Sodium SulfiteHCID 197110Acetic acid mixture with peracetic acidHCID 178463108HCID 178463108, compound

Product 1

HCID 178463106HCID 178463106, compoundYield 77%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6212ChloroformSolvent

Procedure

0.39 Gram (1.2 mmol) of 6-(1-ethyl-5-hydroxypyrazol-4-yl)carbonyl-5,8-dimethylthiochrom-2-en-4-one was dissolved in 4 ml of chloroform, and 0.62 g (2.6 mmol) of a 32 wt % peracetic acid/acetic acid solution was added. The mixture was allowed to react at room temperature for 5 hours, and then allowed to react at 50° C. for 2 hours and further stirred at room temperature for 17 hours. After the reaction, the reaction mixture was diluted with water, and a 1 wt % sodium sulfite aqueous solution was added to decompose excess peracetic acid. An organic substance was extracted with ethyl acetate, washed with a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 0.33 g (yield 77%) of the titled compound. Table 24 shows the physical property data of the titled compound.

Workup

  1. customto react at room temperature for 5 hours
  2. customto react at 50° C. for 2 hours
  3. customAfter the reaction
  4. extractionAn organic substance was extracted with ethyl acetate
  5. washwashed with a saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-02f82193500049619f4f1911fc9938c0
Source dataset
uspto-grants-2000_12
Patent number
US06159904

Reaction notes

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