反応 #742249

ord-6341323ae66147b3b237f867cf3338d6

反応方程式

CCOC(=O)C=P(c1ccccc1)(c1ccccc1)c1ccccc1
ethoxycarbonylmethylenetriphenylphosphorane
Cc1ccccc1
toluene
CCN(CC)c1ccc(C(C)=O)c(O)c1
1-(4-diethylamino-2-hydroxy-phenyl)ethanone
CCOC(=O)C=C(C)c1ccc(N(CC)CC)cc1O
3(4-Diethylamino-2-hydroxy-phenyl)-but-2-enoic acid ethyl ester

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Then the reaction mixture was heated to reflux
  2. 2
    温度After refluxing for 31 hours the mixture
  3. 3
    温度was cooled down
  4. 4
    その他evaporated to dryness
  5. 5
    その他The resulting dark oil was purified by chromatography
  6. 6
    その他to yield a colourless oil

実験手順

To a suspension of 5.27 g ethoxycarbonylmethylenetriphenylphosphorane in 10 ml of toluene, a solution of 2.02 g 1-(4-diethylamino-2-hydroxy-phenyl)ethanone (DE 28 44 606) was dropped in at room temperature. Then the reaction mixture was heated to reflux. After refluxing for 31 hours the mixture was cooled down and evaporated to dryness. The resulting dark oil was purified by chromatography to yield a colourless oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE043006E1uspto-grants-2011_12