反应详情

To a cold solution of sodium hydroxide (9.75 g, 240 mmol) in methanol (200 mL), thioglycollic acid (11.25 g, 120 mmol) was added slowly over 30 minutes. Sodium thioglycollate precipitated was dissolved by stirring and warming up the solution. The solution was cooled to room temperature and 4-methoxy-3-nitrobenzyl chloride (30.0 g, 120 mmol) was added in portions to reduce the intensity of exothermic reaction. The reaction mixture was then refluxed for 4 hours, cooled and poured onto crushed ice (1 Kg) containing hydrochloric acid (50 mL). The precipitate formed was filtered, washed with ice cold water and dried under vacuum. (30.0 g, 95% yield) m.p. 130-132° C.

1. customSodium thioglycollate precipitated
2. dissolutionwas dissolved
3. temperaturewarming up the solution
4. customthe intensity of exothermic reaction
5. temperatureThe reaction mixture was then refluxed for 4 hours
6. temperaturecooled
7. additionpoured
8. customThe precipitate formed
9. filtrationwas filtered
10. washwashed with ice cold water
11. customdried under vacuum