Acetic Acid → HCID 19972358, compound

HRID 1452296Notes

Reaction equation

HRID 1452296 reaction equation
OO.[Cl:3][CH2:4][CH2:5][CH2:6][S: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][CH2:6][S: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

Conditions

Temperature
60 °C

Procedure

7 ml of 30% hydrogen peroxide was added at 20°-25° C. to a solution of 3.65 g of Intermediate XXXIV in 35 ml of acetic acid. After stirring for 4 hours at 60° C., the reaction mixture was cooled to 20°-25° C. 30 ml of water was added. A precipitate formed, and was collected by suction filtration, washed with water and dried, yielding 3.4 g of the title compound. After crystallization from acetone, it showed a melting point of 160°-163° C.

Workup

  1. temperaturethe reaction mixture was cooled to 20°-25° C
  2. customA precipitate formed
  3. filtrationwas collected by suction filtration
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-86152c4530b547a9b3af29803a4e9333
Source dataset
uspto-grants-1997_02
Patent number
US05605896

Reaction notes

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