Methyl 4-chloro-2-(chlorosulphonyl)benzoate → 52948-12-6

HRID 1241238Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1241238
Cl[S:2]([C:5]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=O)=O>Cl.[Zn]>[SH:2][C:5]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]

Komponenten

4

Edukt 1

HCID 3020661Methyl 4-chloro-2-(chlorosulphonyl)benzoate

Produkt 1

HCID 1565712452948-12-6

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. waitAfter 2 hours at this temperature
  2. temperaturethe mixture was cooled
  3. waitto stand at room temperature for 12 hours
  4. extractionextracted with ethyl acetate
  5. customthe combined organic phases were dried
  6. customthe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-cfd27acc07684b6b8c7ec8e9f58ee4c1
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07115545B1

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