Реакция #1328420

ord-cfd27acc07684b6b8c7ec8e9f58ee4c1

Уравнение реакции

COC(=O)c1ccc(Cl)cc1S(=O)(=O)Cl
methyl 2-chlorosulfonyl-4-chlorobenzoate
COC(=O)c1ccc(Cl)cc1S
Methyl 2-mercapto-4-chlorobenzoate

Реагенты

Растворители

Условия реакции

Температура
70°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07115545B1uspto-grants-2006_10