反応 #1119556

ord-7185e3ffd15740eb97b88d274fab1b78

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated
  2. 2
    workup.STIRRINGThe mixture is stirred at 100° C. for two hours
  3. 3
    その他a solvent is removed under reduced pressure
  4. 4
    洗浄The organic phase is washed with water
  5. 5
    その他dried
  6. 6
    濃縮concentrated

実験手順

2.4 g (0.02 mol) of 4-chloro-1-hydroxypyrazole in 30 ml of ethanol are added dropwise to a solution of 1.2 g (0.02 mol) of potassium hydroxide in 50 ml of ethanol. The reaction mixture is stirred at room temperature for two hours and then concentrated. The residue is taken up in 60 ml of dimethylformamide, and 5.7 g (0.02 mol) of methyl α-(2-bromomethylphenyl)-β-methoxyacrylate in 30 ml of dimethylformamide are added. The mixture is stirred at 100° C. for two hours, a solvent is removed under reduced pressure and the residue is taken up in methyl tertbutyl ether. The organic phase is washed with water, dried and concentrated. 5.0 g (77%) of the title compound are obtained as an oil (compound no. 9).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04957937uspto-grants-1990_09