反应详情

A heterogeneous mixture of 3-chlorosulfonyl-benzoic acid (11.0 g, 50.0 mmol) in 18 mL of SOCl2 was refluxed for 3 h. Thereafter the excess of SOCl2 was removed, the residual brown oil was dissolved in 60 mL of CH3CN, and then 2-(p-tolylsulfonyl)ethanol (9.4 g, 47.0 mmol, 0.95 eq.) was added. The mixture was heated to reflux temperature for 20 h. Thereafter the most of CH3CN was removed, the resulting oil was purified by short column chromatography (silica gel, CH2Cl2) to give light brown oil, which was dried further under vacuum to yield 19.1 g (95%) of a light brown solid.

1. temperaturewas refluxed for 3 h
2. customThereafter the excess of SOCl2 was removed
3. dissolutionthe residual brown oil was dissolved in 60 mL of CH3CN
4. temperatureThe mixture was heated
5. temperatureto reflux temperature for 20 h
6. customThereafter the most of CH3CN was removed
7. customthe resulting oil was purified by short column chromatography (silica gel, CH2Cl2)
8. customto give light brown oil, which
9. customwas dried further under vacuum