Chlorosulfonic acid → HCID 15051878, compound
Reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH3:6][O:7][CH2:8][CH2:9][C:10]1[CH:14]=[CH:13][S:12][CH:11]=1>>[CH3:6][O:7][CH2:8][CH2:9][C:10]1[CH:14]=[CH:13][S:12][C:11]=1[S:2]([Cl:1])(=[O:5])=[O:3]Participants
3
Conditions
- Temperature
- -10 °C
Procedure
To 56 g of chlorosulfonic acid at -15° C. was added with efficient stirring 14.2 g of 3-(2-methoxyethyl)thiophene. The mixture was stirred for one hour at -10° C. and then cautiously added to ice and the resultant mixture extracted with methylene chloride. The methylene chloride extract was washed with cold water, dried over magnesium sulfate, filtered and concentrated to yield 6.0 g of an oil. Infrared absorption spectroscopy showed peaks at 1160, 1180 and 1360 cm-1 consistent for sulfonyl chloride. This product was sufficiently pure for use as an intermediate for the preparation of compounds of this invention.
Workup
- additioncautiously added to ice
- extractionthe resultant mixture extracted with methylene chloride
- extractionThe methylene chloride extract
- washwas washed with cold water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-60666220c11740399a84440182659f47
- Source dataset
- uspto-grants-1989_10
- Patent number
- US04877440
Reaction notes
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