Reaktion #1328420

Reaktionsgleichung

methyl 2-chlorosulfonyl-4-chlorobenzoate

→

Methyl 2-mercapto-4-chlorobenzoate

Lösungsmittel

hydrochloric acid

—

ice

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITAfter 2 hours at this temperature
2. 2
   Temperaturthe mixture was cooled
3. 3
   workup.WAITto stand at room temperature for 12 hours
4. 4
   Extraktionextracted with ethyl acetate
5. 5
   Sonstigethe combined organic phases were dried
6. 6
   Sonstigethe solvent was removed

Vorschrift

Over a period of 1.5 hours, 243.5 g (3.7 mol) of zinc powder were added a little at a time to a suspension of 205 g (0.75 mol) of methyl 2-chlorosulfonyl-4-chlorobenzoate in 1 l of concentrated hydrochloric acid and 375 g of ice. The mixture was stirred for another 3 hours and slowly heated to 70° C. After 2 hours at this temperature, the mixture was cooled. The reaction mixture was allowed to stand at room temperature for 12 hours and then extracted with ethyl acetate, the combined organic phases were dried and the solvent was removed. This gave 125.4 g (83%) of methyl 2-mercapto-4-chlorobenzoate.

Quelle