반응 #352773

반응 방정식

mannitol

sodium ethylate

acryloyl chloride

→

mannitol diacrylate

용매

n-hexane

methanol

methanol

반응 조건

후처리

1. 1
   workup.DISSOLUTIONis subsequently dissolved
2. 2
   온도in reflux
3. 3
   온도in reflux for one hour
4. 4
   기타is formed
5. 5
   기타Methanol is then evaporated off in a vacuum
6. 6
   workup.ADDITIONthe mixture is mixed to an emulsion four times in n-hexane
7. 7
   기타once again the solvent is removed
8. 8
   기타the mixture is dried in a desiccator
9. 9
   기타11.5 g of a light yellow crystaline substance is obtained
10. 10
    기타(Merck, stabilised for synthesis)
11. 11
    기타the mixture is dried in a vacuum

실험 절차

9.1 g mannitol (D(-)-Mannitol, Merck, for determination of boric acid) is mixed to an emulsion in 120 ml methanol (Merck, dried for analysis purposes) in a round flask, and is subsequently dissolved through boiling in reflux. 18 g of sodium ethylate is then slowly added (Merck, 30% in methanol) and boiled in reflux for one hour. A felt of long needles is formed. Methanol is then evaporated off in a vacuum and the mixture is mixed to an emulsion four times in n-hexane and once again the solvent is removed and the mixture is dried in a desiccator. 11.5 g of a light yellow crystaline substance is obtained. This is mixed to an emulsion in 120 ml n-hexane in a 250 ml round flask and maintained at 17 degrees C. Under heavy agitation, 9.1 g acryloyl chloride is slowly added (Merck, stabilised for synthesis). After 5 hours of agitation and 10 hours standing, 0.1 g of hydroquinone is added and the mixture is dried in a vacuum. 21.3 g of a mannitol diacrylate and common salt mixture is formed. The mixture is dissolved in 200 ml deionised water and subsequently, by means of an ion exchanger, (Amberlite IR 120, acidic) separated from the common salt. 0.1 g hydroquinone is introduced into the eluate, the water is removed and drying in a desiccator is then undertaken. 15.3 g of a light yellow substance remains. This is completely soluble in water or in acrylic acid. It is hard to dissolve in acetone, methanol, ethanol or ethyl acetate.

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