HRID1025253
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperaturerefluxed for 5 hours
- customAfter evaporating the solvent
- dissolutionthe residue was dissolved in 1000 g of dehydrated methanol
- temperaturethe mixture was heated
- temperaturerefluxed for 5 hours
- customAfter evaporating the solvent
- dissolutionthe residue was dissolved in 300 g of n-hexane
- filtrationThe solution was filtered through 50 g of silica gel
- customto remove DMAP