Reaktion #498458

Reaktionsgleichung

carbobenzoxychloride

sodium hydrogen carbonate

HCl

4-Amino-3-methylbenzoic acid

carbobenzoxychloride

sodium hydrogen carbonate

→

product

Ausbeute 45.3%

N-Carbobenzoxy-4-amino-3-methylbenzoic Acid

Ausbeute 45.3%

Lösungsmittel

ether

water

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder cooling with ice
2. 2
   Temperaturunder cooling with ice
3. 3
   workup.STIRRINGthe mixture was stirred for 1.5 h at room temperature
4. 4
   Filtrationthe separating insoluble matter was recovered by filtration
5. 5
   SonstigeThe recovered solids were vacuum-dried

Vorschrift

4-Amino-3-methylbenzoic acid (5.0 g) was suspended in water (80 ml) and, thereafter, an ether solution (20 ml) of carbobenzoxychloride (3.7 g) and sodium hydrogen carbonate (3.6 g) were alternately added to the suspension under cooling with ice. Following stirring for 2.5 h at room temperature, an ether solution (95 ml) of carbobenzoxychloride (3.7 g) and sodium hydrogen carbonate (7.2 g) were further added alternately under cooling with ice, and the mixture was stirred for 1.5 h at room temperature. After rendering the reaction solution acidic with 4N HCl, the separating insoluble matter was recovered by filtration. The recovered solids were vacuum-dried to yield the end product (2.8 g).

Quelle