Acetic Acid → HCID 14324494, compound

HRID 1588379Notes

Reaction equation

HRID 1588379 reaction equation
[Na].[CH2:2]([S:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][C:14]=1[N+:23]([O-:25])=[O:24])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].C(O)(=[O:28])C.OO.[OH2:32]>>[CH2:2]([S:12]([C:13]1[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][C:14]=1[N+:23]([O-:25])=[O:24])(=[O:28])=[O:32])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]

Participants

6

Reactant 5

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 5360545SodiumHCID 14324493HCID 14324493, compound

Product 1

HCID 14324494HCID 14324494, compoundYield 99.3%

Procedure

After adding 1 g of sodium tungstenate to a mixture of 86 g of 4-decylthio-3-nitrobenzotrifluoride obtained in the above step and 300 ml of acetic acid, the resultant mixture was heated to 70° C. Then, 46 ml of an aqueous 35% hydrogen peroxide solution was added dropwise to the mixture while maintaining it at 80° to 85° C. Thereafter, the reaction was performed for 6 hours at the same temperature. After the reaction was over, water was added to the reaction mixture and crystals thus deposited were recovered by filtration and dried to provide 93.1 g of the desired product with a yield of 99.3%.

Workup

  1. temperaturewhile maintaining it at 80° to 85° C
  2. additionwas added to the reaction mixture and crystals
  3. filtrationthus deposited were recovered by filtration
  4. customdried

Sources & evidence

ORD record
ord-ca36ed2f69794627a0cc067a01a7d5b5
Source dataset
uspto-grants-1993_06
Patent number
US05221750

Reaction notes

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