Reaktion #1796895

Reaktionsgleichung

Dipropylene glycol monomethyl ether

benzoic acid

toluene

→

desired product

Ausbeute 91.8%

Dipropylene Glycol Monomethyl Ether Benzoate

Ausbeute 91.8%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with stirrer
2. 2
   SonstigeThe reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours
3. 3
   SonstigeDuring that time, water (44 mls) was removed
4. 4
   Sonstigefor 2.5 hours
5. 5
   Sonstigeat 224°-226° C.
6. 6
   Sonstigewith the removal of water (56 mls.)
7. 7
   WaschenThe reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%)
8. 8
   Waschenwashed with water (400 ml)
9. 9
   workup.ADDITIONThen additional water (200 ml) was added
10. 10
    Sonstigethe product separated
11. 11
    Sonstigedried at 125°
12. 12
    Filtrationfiltered

Vorschrift

Dipropylene glycol monomethyl ether (444.6 grams; 3.0 mol), benzoic acid (373.7 grams; 3.06 mol), toluene (50 ml) and zirconium carbonate (2.0 grams) were placed into a 200 ml, 3-necked round bottom flask equipped with stirrer, thermometer, heating mantle, Dean Stark water trap, condenser and 10" Vigneux column. The reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours with stirring. During that time, water (44 mls) was removed. The reaction was continued the next day for 2.5 hours at 224°-226° C. with the removal of water (56 mls.). The reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%) and then washed with water (400 ml). Then additional water (200 ml) was added and the product separated and dried at 125°, cooled to 100° C. and filtered. The desired product (694.6 grams) was obtained representing a yield of 91.8%. It assayed 99.5% with the following properties:

Quelle