HRID1025253

反应详情

EQUATION

反应方程式

HRID 1025253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperaturerefluxed for 5 hours
  3. customAfter evaporating the solvent
  4. dissolutionthe residue was dissolved in 1000 g of dehydrated methanol
  5. temperaturethe mixture was heated
  6. temperaturerefluxed for 5 hours
  7. customAfter evaporating the solvent
  8. dissolutionthe residue was dissolved in 300 g of n-hexane
  9. filtrationThe solution was filtered through 50 g of silica gel
  10. customto remove DMAP