Reaktion #1112435

Reaktionsgleichung

ethyl 2,2-difluoro-3-(methacryloyloxy)pentanoate

→

methyl 2,2-difluoro-3-(methacryloyloxy)pentanoate

Ausbeute 95.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturrefluxed for 5 hours
3. 3
   SonstigeAfter evaporating the solvent
4. 4
   workup.DISSOLUTIONthe residue was dissolved in 1000 g of dehydrated methanol
5. 5
   Temperaturthe mixture was heated
6. 6
   Temperaturrefluxed for 5 hours
7. 7
   SonstigeAfter evaporating the solvent
8. 8
   workup.DISSOLUTIONthe residue was dissolved in 300 g of n-hexane
9. 9
   FiltrationThe solution was filtered through 50 g of silica gel
10. 10
    Sonstigeto remove DMAP

Vorschrift

100 g of ethyl 2,2-difluoro-3-(methacryloyloxy)pentanoate was dissolved in 1000 g of dehydrated methanol in a nitrogen atmosphere. After the addition of 0.1 g of N,N-dimethylaminopyridine (DMAP), the mixture was heated and refluxed for 5 hours. After evaporating the solvent, the residue was dissolved in 1000 g of dehydrated methanol, and the mixture was heated and refluxed for 5 hours. After evaporating the solvent, the residue was dissolved in 300 g of n-hexane. The solution was filtered through 50 g of silica gel to remove DMAP. 89.7 g of methyl 2,2-difluoro-3-(methacryloyloxy)pentanoate (M-29) was thus obtained (yield: 95%).

Quelle