反応 #165928

ord-cef9affb204c4359a1873eeea5425a27

反応条件

温度
7.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reaction mass
  2. 2
    温度by maintaining temp below 10° C
  3. 3
    その他Reaction mass
  4. 4
    その他Reaction mass
  5. 5
    洗浄was washed with sodium bicarbonate solution (8%, 3×400 ml)
  6. 6
    その他Reaction mass
  7. 7
    濃縮was then concentrated to residue

実験手順

Ethyl-2-(4,5-dihydrofuran-3-yl)-2-oxoacetate (100 g) was dissolved in dichloromethane (500 ml) and Ethanol (150 ml) was added to reaction mass and then reaction mass was cooled to 5 to 10° C. N-bromosuccinimide (115 g) was added lot wise by maintaining temp below 10° C. Reaction mass was then stirred at 20-30° C. till completion of reaction. Reaction mass was washed with sodium bicarbonate solution (8%, 3×400 ml). Reaction mass was then concentrated to residue to get Ethyl-2-(3-bromo-2-ethoxytetrahydrofuran-3-yl)-2-oxoacetate (Yield 170 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841467B2uspto-grants-2014_09