Chloroform → Methyl 4-amino-3,5-dichlorobenzoate

HRID 1441041Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1441041
[NH2:1][C:2]1C=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.S(Cl)([Cl:15])(=O)=O.[OH-].[Na+].[CH:19]([Cl:22])(Cl)Cl>>[NH2:1][C:2]1[C:3]([Cl:15])=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:19]=1[Cl:22]

Komponenten

5

Versuchsvorschrift

Methyl 4-aminobenzoate (25 g.) in dry chloroform (250 ml.) was treated dropwise with sulphuryl chloride (10 ml.) and the mixture heated at reflux for 4 hours. A further supply of sulphuryl chloride (10 ml.) was added and heating continued for a further 2 hours. The reaction mixture was poured onto ice and 2N sodium hydroxide solution was added. The organic solution was separated and the aqueous phase extracted with ethyl acetate. The combined organic solution was dried (anhydrous magnesium sulphate) and evaporated to give methyl 4-amino-3,5-dichlorobenzoate as a solid.

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureat reflux for 4 hours
  3. temperatureheating
  4. additionwas added
  5. customThe organic solution was separated
  6. extractionthe aqueous phase extracted with ethyl acetate
  7. dry with materialThe combined organic solution was dried (anhydrous magnesium sulphate)
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d5b8192b3b144b0399836676248d826a
Quelldatensatz
uspto-grants-1996_03
Patentnummer
US05502073

Notizen zur Reaktion

Wird geladen…