Carbon Tetrachloride → HCID 20384180, compound
Reaction equation
[C:1]([C:4]1[CH:17]=[CH:16][C:15]2[O:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7](=[O:19])(=[O:18])[C:6]=2[CH:5]=1)([OH:3])=[O:2].S(Cl)(Cl)=O.[C:24](Cl)(Cl)(Cl)Cl>>[CH3:24][O:2][C:1]([C:4]1[CH:17]=[CH:16][C:15]2[O:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7](=[O:19])(=[O:18])[C:6]=2[CH:5]=1)=[O:3]Participants
4
Procedure
2-Carboxyphenoxathiin-10,10-dioxide, (0.50 g.) in carbon tetrachloride (25 ml.) and thionyl chloride (2.0 ml.) was boiled under reflux for 2 hr. The solvent was evaporated and methanol (20 ml.) added. The mixture was boiled under reflux for 20 min., and cooled, whereupon 2-methoxycarbonylphenoxathiin-10,10-dioxide crystallised out and was filtered off and dried, m.pt. 160° C.
Workup
- temperatureunder reflux for 2 hr
- customThe solvent was evaporated
- additionmethanol (20 ml.) added
- temperatureunder reflux for 20 min.
- temperaturecooled, whereupon 2-methoxycarbonylphenoxathiin-10,10-dioxide
- customcrystallised out
- filtrationwas filtered off
- customdried
Sources & evidence
- ORD record
- ord-485996e6b99345c38ab1dc8ff1c0a0b1
- Source dataset
- uspto-grants-1979_12
- Patent number
- US04177257
Reaction notes
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