تفاعل #1328420

ord-cfd27acc07684b6b8c7ec8e9f58ee4c1

معادلة التفاعل

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

الكواشف

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07115545B1uspto-grants-2006_10