Hydrochloric Acid → Ethyl 6-chloropicolinate

HRID 706721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 706721
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1.Cl.[CH3:12][CH2:13]O>>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH2:12][CH3:13])=[O:9])[CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 208126-Chloropicolinic acid

Produkt 1

HCID 11063114Ethyl 6-chloropicolinateAusbeute 85 %

Versuchsvorschrift

To 6-chloropicolinic acid (5.01 g, 31.8 mmol) in EtOH (100 mL) was added concentrated HCl (6 mL, 78 mmol). The reaction was heated to reflux for overnight, cooled to ambient temperature and concentrated under reduced pressure. The residue was dissolved in DCM (100 mL) and NaOH (2M) aqueous solution was added until pH=8. The aqueous layer was then extracted with DCM. The combined organic extracts were combined, dried (Na2SO4) and concentrated under reduced pressure to give the desired product (85%).

Aufarbeitung

  1. temperatureThe reaction was heated
  2. temperatureto reflux for overnight
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in DCM (100 mL)
  5. additionNaOH (2M) aqueous solution was added until pH=8
  6. extractionThe aqueous layer was then extracted with DCM
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-336a65bc60514981b4cbbb45292c4bf7
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09174981B2

Notizen zur Reaktion

Wird geladen…