Acetic Acid → HCID 19972680, compound
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
Conditions
- Temperature
- 60 °C
Procedure
41.6 ml of 30% hydrogen peroxide was added dropwise at 40° C. over a period of 20 minutes to a solution of 26.2 g of Intermediate XII in 300 ml of glacial acetic acid. The mixture was heated at 60° C. with stirring for 4.5 hours, then cooled to ambient temperature and poured into 60 ml of water. Suction filtration gave a solid which was washed with water and dried, to give 29.4 g of the title compound. Melting point 158°-161° C. (ethanol).
Workup
- temperaturecooled to ambient temperature
- filtrationSuction filtration
- customgave a solid which
- washwas washed with water
- customdried
Sources & evidence
- ORD record
- ord-a176b79b0f11468282438aed4962d0f5
- Source dataset
- uspto-grants-1995_09
- Patent number
- US05453518
Reaction notes
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