Hydrochloric Acid → Methyl(4-aminophenoxy)acetate

HRID 1882310

Reaktionsgleichung

Reaktionsgleichung von HRID 1882310
Cl.[NH2:2][C:3]1[CH:13]=[CH:12][C:6]([O:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:5][CH:4]=1.Cl.[CH3:15]O>>[CH3:15][O:10][C:9](=[O:11])[CH2:8][O:7][C:6]1[CH:5]=[CH:4][C:3]([NH2:2])=[CH:13][CH:12]=1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 668114882-(4-Aminophenoxy)acetic acid hydrochloride

Produkt 1

HCID 6422115Methyl(4-aminophenoxy)acetateAusbeute 58,5 %

Versuchsvorschrift

To a mixture (4-Amino-phenoxy)acetic acid HCl 60 (250 grams, 1.228 mol), in methanol (5 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 10 hours. Methanol (3.5 liters) was distilled and ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 61 was filtered, dried, and recrystallized from a mixture of Chloroform:Hexane (1:5) to give pure 61 (130 grams, 58.5%) as a light brown powder The melting point was found to be 65-66.8° C.

Aufarbeitung

  1. customat 10° C.
  2. customfor 1 hour
  3. temperaturerefluxed for 10 hours
  4. distillationMethanol (3.5 liters) was distilled
  5. additionice water (1 liter) was added
  6. filtrationCrude 61 was filtered
  7. customdried
  8. customrecrystallized from a mixture of Chloroform:Hexane (1:5)

Quellen und Nachweise

ORD-Eintrag
ord-a035ee5898114d57826ef170fccf823c
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08318973B2

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