Reaktion #1483129

Reaktionsgleichung

squaric acid

2-(methyl(3-acetaminophenyl)amino)ethan-1-ol

n-BuOH

→

desired compound

2,4-bis(2-acetamino-4-((2-hydroxyethyl)(methyl)amino)phenyl)cyclobuta-1,3-dien-1,3-diol

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated
2. 2
   Sonstigeto remove water
3. 3
   Sonstigegenerated during the reaction
4. 4
   Sonstigethe reactant kept being reacted
5. 5
   Temperaturthe reactant was cooled down
6. 6
   Sonstigeproducing crystals
7. 7
   FiltrationThe crystals were filtered
8. 8
   Sonstigeonce more recrystallized

Vorschrift

342 mg of squaric acid and 2 g of 2-(methyl(3-acetaminophenyl)amino)ethan-1-ol were put in a 100 mL 3-neck rounded bottom flask, and 40 mL of n-BuOH and 20 mL of toluene were added thereto. The mixture was heated and refluxed at 120° C. for 10 hours. Next, a Dean-Stark trap set was used to remove water generated during the reaction, and the reactant kept being reacted. When the reaction was complete, the reactant was cooled down, producing crystals. The crystals were filtered, several times cleaned with hexane, and once more recrystallized, obtaining a desired compound.

Quelle