反応 #6566

ord-10fea42bec564443a9bc5ae1ea51daad

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After heating
  2. 2
    温度under reflux for 4 hours
  3. 3
    洗浄washed with ether
  4. 4
    抽出extracted 4 times with ether
  5. 5
    乾燥The organic phase was dried over sodium sulphate
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated in a rotary evaporator

実験手順

5.56 g (99 mmol) KOH flakes were dissolved in 6.82 ml water and 13.65 ml ethanol and then treated with 11.12 g (28.34 mmol) of dibenzyl 2-(3,4,4-trifluoro-3-butenyl)-malonate. After heating under reflux for 4 hours, the reaction mixture was poured into 30 ml water and washed with ether. The aqueous phase was acidified with dilute hydrochloric acid and extracted 4 times with ether. The organic phase was dried over sodium sulphate, filtered and then concentrated in a rotary evaporator.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05248810uspto-grants-1993_09