Reaktion #1483126

Reaktionsgleichung

squaric acid

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

n-BuOH

→

desired compound

2,4-bis(2-n-butoxy-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 from the reactant during the reaction
4. 4
   Sonstigekept being reacted
5. 5
   Temperaturthe reactant was cooled down
6. 6
   Sonstigeproducing crystals
7. 7
   FiltrationThe crystals was filtered
8. 8
   Waschenseveral times washed with hexanes
9. 9
   Sonstigeonce more recrystallized

Vorschrift

342 mg of squaric acid and 2.14 g of 2-(methyl(3-butoxyphenyl)amino)ethan-1-ol was put in a 100 mL 3-necked round 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 7 hour. Then, a Dean-Stark trap set was used to remove water generated from the reactant during the reaction and kept being reacted. When the reaction was complete, the reactant was cooled down, producing crystals. The crystals was filtered, several times washed with hexanes, and once more recrystallized, obtaining a desired compound.

Quelle