Reaktion #216536

Reaktionsgleichung

acrylic acid

diethylene glycol monobutyl ether

C4F9SO2N(H)C3H6N(CH3)2

acrylic acid

phenothiazine

→

C4F9SO2N(C2H4COOH)C3H6N(CH3)2

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with an air stirrer
2. 2
   Sonstigeto react for 6 hours
3. 3
   SonstigeAfter this reaction period
4. 4
   workup.ADDITIONWhile still mixing
5. 5
   Temperaturto cool to room temperature

Vorschrift

An acrylic acid Michael addition reaction was then run according to the general procedure given in U.S. Pat. No. 5,144,069 (Stern et al.). 50 g (0.12 mole) of the purified C4F9SO2N(H)C3H6N(CH3)2, 16.4 g (0.23 mole) of acrylic acid and 0.2 g of phenothiazine (free radical polymerization inhibitor) were added to a 250-mL three-neck flask equipped with an air stirrer and thermometer. The resulting mixture was heated to 125° C. and was allowed to react for 6 hours. After this reaction period, a positive solubility check of the product in water of pH 7 indicated that the Michael addition reaction was essentially complete. While still mixing, a solvent blend of 18 g of diethylene glycol monobutyl ether and 42 g of deionized water was added and the mixture was allowed to cool to room temperature. The water solubility test was run again with the same positive result, showing good conversion to the desired Michael addition product, C4F9SO2N(C2H4COOH)C3H6 (CH3)2.

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