反応 #61525

ord-4c8badb3b96b4d3aa4e6dc9d0f230fe0

反応方程式

Cl
hydrochloric acid
CC(=O)c1ccco1
1-furan-2-yl-ethanone
CCOC(=O)C(=O)OCC
oxalic acid diethyl ester
CC(C)(C)[O-].[K+]
KOt-Bu
CCOC(=O)C(=O)CC(=O)c1ccco1
4-Furan-2-yl-2,4-dioxo-butyric acid ethyl ester

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic layer was separated
  2. 2
    洗浄washed with 150 ml water
  3. 3
    乾燥dried over MgSO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他to yield a white solid

実験手順

To a solution of 16 g oxalic acid diethyl ester in 350 ml THF, 10.1 g KOt-Bu were added at 0° C. Then 10 g 1-furan-2-yl-ethanone in 50 ml THF were added dropwise. After 1 h the reaction mixture was diluted with 300 ml ethyl acetate and 200 mnl water. This solution was acidified with diluted hydrochloric acid to pH 5. The organic layer was separated, washed with 150 ml water, dried over MgSO4, filtered and concentrated under reduced pressure to yield a white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07429581B2uspto-grants-2008_09