Reaktion #166048

Reaktionsgleichung

acetic anhydride

Tranexamic acid

sulfuric acid

acetic anhydride

water

→

trans-{4-[(acetylamino) methyl]cyclohexyl}carboxylic acid

Ausbeute 98.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
2. 2
   EinengenThe reaction solution was concentrated under reduced pressure
3. 3
   Sonstigethe residue was further azeotroped with toluene
4. 4
   SonstigeThe resulting precipitates
5. 5
   Filtrationwere collected by filtration
6. 6
   Waschenwashed with ether
7. 7
   Sonstigedried under reduced pressure

Vorschrift

Tranexamic acid (10 g, 63.6 mmol) was suspended in acetic anhydride (50 mL), this suspension was added with concentrated sulfuric acid (0.01 mL) at room temperature, and the mixture was stirred overnight at the same temperature. Under ice cooling, the reaction mixture was added with water (100 mL), and the mixture was stirred at room temperature for 1 hour to decompose excess acetic anhydride. The reaction solution was concentrated under reduced pressure, and the residue was further azeotroped with toluene. The resulting precipitates were collected by filtration, washed with ether, and dried under reduced pressure to obtain trans-{4-[(acetylamino) methyl]cyclohexyl}carboxylic acid as white solid (12.46 g, 98%).

Quelle