反应详情

To a 5-liter flask equipped with a mechanical stirrer and reflux condenser was added p-toluenesulfinic acid, lithium salt (308.57 g), N-(2-sulfoethyl)-2-bromoacetamide, lithium salt (527.39 g), water (180 ml), and ethyl alcohol (3380 ml). The resulting suspension was heated to reflux. After about an hour of reflux, nearly all of the reactants had dissolved. Reflux was continued another four hours, and the solution was filtered hot through a Celite pad to remove some haziness. The solution was cooled overnight to room temperature. The solid that formed was collected and washed with 1 liter of 95% ethyl alcohol/water. The white solid was air dried and then dried at high vacuum, providing 553.88 g (89% yield) of 2-(4-methylphenyl)sulfonyl-N-(2-sulfoethyl)acetamide, lithium salt (Intermediate 1). HPLC analysis showed no detectable impurities. Ion chromatography indicated 0.035 weight % bromide and 1.8 weight % lithium. The material exhibited an acceptable proton spectrum.

1. customTo a 5-liter flask equipped with a mechanical stirrer
2. temperaturereflux condenser
3. temperatureThe resulting suspension was heated to reflux
4. temperatureAfter about an hour of reflux
5. dissolutionnearly all of the reactants had dissolved
6. temperatureReflux
7. filtrationthe solution was filtered hot through a Celite pad
8. customto remove some haziness
9. temperatureThe solution was cooled overnight to room temperature
10. customThe solid that formed
11. customwas collected
12. washwashed with 1 liter of 95% ethyl alcohol/water
13. customdried
14. customdried at high vacuum