Ethanol → Ethyl 4-amino-3-methylbenzoate

HRID 1498897

Reaktionsgleichung

Reaktionsgleichung von HRID 1498897
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[CH3:11].[CH2:12](O)[CH3:13]>S(=O)(=O)(O)O>[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:12][CH3:13])=[O:7])=[CH:4][C:3]=1[CH3:11]

Komponenten

4

Edukt 2

HCID 702EthanolHCID 755984-Amino-3-methylbenzoic acid

Produkt 1

HCID 282796Ethyl 4-amino-3-methylbenzoateAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

To a suspension of 4-amino-3-methylbenzoic acid (5.00 g, 33.1 mmol) in ethanol (50 ml), concentrated sulfuric acid (5.00 ml) was slowly added. The mixture was heated under reflux for 3 hours. The solvent was distilled off under a reduced pressure. After the volume of the mixture was approximately halved, the mixture was neutralized with a saturated sodium bicarbonate solution. The mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated to give the title compound (5.87 g, 99%) as a light-brown solid.

Aufarbeitung

  1. additionwas slowly added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. distillationThe solvent was distilled off under a reduced pressure
  5. extractionThe mixture was subjected to extraction with ethyl acetate
  6. dry with materialthe extract was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-d61fe132b4f64063afa55e42e5285956
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09200008B2

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