反应 #70126

ord-ae4ed1cf31ce486a998b94fc968f4a3b

反应方程式

C=C(C)C(=O)Cl
methacrylic acid chloride
CCC1(O)CCC(F)(F)CC1
1-ethyl-4,4-difluorocyclohexanol
CCN(CC)CC
triethylamine
C=C(C)C(=O)OC1(CC)CCC(F)(F)CC1
1-ethyl-4,4-difluorocyclohexyl methacrylate
收率 79.9%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A four-necked flask equipped with a stirrer
  2. 2
    其他to obtain a solution
  3. 3
    其他A solution prepared
  4. 4
    workup.ADDITIONwas added to the solution at 4° C. over 30 minutes
  5. 5
    workup.STIRRINGThe mixture was stirred at 4° C. for 3 hours
  6. 6
    其他to obtain a reaction mixture
  7. 7
    洗涤The reaction mixture was washed with water

实验过程

A four-necked flask equipped with a stirrer, a thermometer, and a dropping funnel was charged with 6.6 g (0.04 mol) of 1-ethyl-4,4-difluorocyclohexanol, 0.2 g of 4-dimethylaminopyridine, 4.9 g of triethylamine, and 20 g of acetone. The mixture was stirred to obtain a solution. A solution prepared by dissolving 4.6 g (0.044 mol) of methacrylic acid chloride in 5 g of acetone was added to the solution at 4° C. over 30 minutes. The mixture was stirred at 4° C. for 3 hours to obtain a reaction mixture. The reaction mixture was washed with water to obtain 7.42 g of 1-ethyl-4,4-difluorocyclohexyl methacrylate (hereinafter may be referred to as “compound (M-8)” ((M-8) in Table 1)). The yield of 1-ethyl-4,4-difluorocyclohexyl methacrylate with respect to 1-ethyl-4,4-difluorocyclohexanol was 78%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08535871B2uspto-grants-2013_09