Acetic Acid → HCID 19972680, compound

HRID 1452288Notes

Reaction equation

HRID 1452288 reaction equation
OO.[Cl:3][CH2:4][CH2:5][S:6][CH2:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1.[OH2:26].C(O)(=[O:29])C>>[Cl:3][CH2:4][CH2:5][S:6]([CH2:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1)(=[O:29])=[O:26]

Participants

5

Reactant 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 19972533HCID 19972533, compound

Product 1

HCID 19972680HCID 19972680, compound

Conditions

Temperature
60 °C

Procedure

41.6 ml of aqueous 30% hydrogen peroxide was added dropwise at 40° C. over a period of 20 minutes to a solution of 26.2 g of Intermediate XXI in 300 ml of glacial acetic acid. The mixture was heated to 60° C., stirred at that temperature for 4.5 hours, cooled to ambient temperature and poured into 60 ml of water. Filtration on a Buchner funnel gave a filter cake which was washed with water and desiccated, yielding 29.4 g of the title compound. A sample was crystallized from ethanol. m.p. (89) 159°-161° C.

Workup

  1. temperaturecooled to ambient temperature
  2. filtrationFiltration on a Buchner funnel
  3. customgave a filter cake which
  4. washwas washed with water

Sources & evidence

ORD record
ord-d335f853a4024fee949d6e9029887851
Source dataset
uspto-grants-1997_02
Patent number
US05605896

Reaction notes

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